CN114259998A - Preparation method of two-dimensional material composite aerogel for rhenium adsorption - Google Patents
Preparation method of two-dimensional material composite aerogel for rhenium adsorption Download PDFInfo
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Abstract
The invention belongs to the technical field of material synthesis, and particularly relates to a preparation method of a two-dimensional material composite aerogel for rhenium adsorption, which is prepared from LiF and Ti2Preparing a two-dimensional material nano-sheet TCNS colloidal solution by using AlC and PDDA as raw materials, and dropwise adding a PDDA aqueous solution into the TCNS colloidal solution under vigorous stirring to synthesize Ti2CT nanosheet/PDDA composite TCNS-P, and then TCNS-P black aerogel cake is obtained, and the prepared two-dimensional material composite aerogel is subjected to rhenium element adsorption test, so that the method has the advantages of high selectivity, high yield, small dosage, low cost, no environmental pollution and recycling.
Description
Technical Field
The invention belongs to the technical field of material synthesis, and particularly relates to a preparation method of a two-dimensional material composite aerogel for rhenium adsorption.
Background
Aerogels are also known as xerogels. When most of the solvent is removed from the gel, the liquid content in the gel is much less than the solid content, or the space network structure of the gel is filled with gas and the appearance is solid. As the lightest solid in the world, the genius world record has been selected. The density of the new material is only 3.55 kilograms per cubic meter and is only 2.75 times of the density of air; the dry pine density (500 kilograms per cubic meter) is 140 times greater than it.
Aerogels are now utilized in many fields. As a heat insulation material, the composite material can effectively transmit sunlight and prevent infrared heat radiation of ambient temperature, is an ideal transparent heat insulation material and has been applied to the aspects of solar energy utilization and building energy conservation. In the aspect of energy storage devices, due to the fact that quantum dot structures are formed in the nano-network of the silicon aerogel, the results of Si doping by a chemical vapor infiltration method and C60 doping by a solution method show that the dopant exists in the form of nano-crystalline grains, and strong visible light emission is observed, so that strong evidence is provided for quantum confinement effect luminescence of the porous silicon. Can also be used for manufacturing space suits, has the function of bulletproof and can treat ecological disasters. The millet is put on an aerogel windproof and water-repellent heat energy coat which is sold after 12 months and 3 days, and is called to have a warm-keeping black technology. Can insulate against cold and high temperatures. The clothes look like weak but not prohibited from wind, and have the same warming effect as thick feather line clothes.
The limited resources make rhenium one of the rarest metal resources in the earth's crust. Some ores contain traces of rhenium, which can only be extracted as a by-product when these ores are processed. This makes it even more important to help re-flow this rare element into the production field by recovering the rhenium-containing material. In recovering precious metals, ensuring stable quality and purity requires profound expertise.
Aerogel is used as a leading-edge novel material, research on rhenium adsorption is less, and a development path of the aerogel on rhenium element adsorption is developed and a good effect is achieved.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a method for preparing a two-dimensional composite aerogel for rhenium adsorption, in which Ti is synthesized by dropwise adding PDDA aqueous solution into TCNS colloidal solution under vigorous stirring2The TCNS-P black aerogel cake is obtained by the CT nanosheet/PDDA compound TCNS-P, and the prepared two-dimensional material composite aerogel is subjected to a rhenium element adsorption test, so that the method has the advantages of high selectivity, high yield, small using amount, low cost, no environmental pollution and recycling.
The invention adopts the following technical scheme:
a preparation method of a two-dimensional material composite aerogel for rhenium adsorption comprises the following steps:
1) preparing a two-dimensional material: adding LiF into hydrochloric acid, stirring until the solution is transparent, and adding Ti2Heating the mixed solution of AlC powder, stirring and reacting at a constant temperature; washing the product with deionized water, and centrifuging at 3000-; repeating the washing and centrifugation cycles until a stable deep red supernatant is obtained; adding deionized water into the supernatant, shaking, centrifuging at 2000-;
2) preparing aerogel: PDDA (M) was added with vigorous stirringw100000-; after the dropwise addition, the mixture is further stirred for 2-3hr (hours) under the inert atmosphere; centrifuging at 10000-; repeating the centrifuging and deionized water washing operations 3-4 times, thus cycling many times to remove excess PDDA; freeze-drying the washed product to obtain black aerogel cake TCNS-P (namely, Ti-containing two-dimensional material composite aerogel for absorbing rhenium)2CT nanosheet/PDDA composite, namely aerogel compounded with two-dimensional materials.
In the preparation method of the two-dimensional material composite aerogel for rhenium adsorption, preferably, in the preparation step of the two-dimensional material, the concentration of hydrochloric acid is 7.5-8.5M, the reaction temperature is 35-45 ℃, and the time is 48-72 hr.
In the preparation method of the two-dimensional material composite aerogel for absorbing rhenium, preferably, in the step of preparing the two-dimensional material, LiF and Ti2The molar ratio of AlC is 1: 1.0-1.1.
In the preparation method of the rhenium adsorption two-dimensional material composite aerogel, preferably, in the aerogel preparation step, PDDA (M)w100000-.
In the preparation method of the two-dimensional composite aerogel for rhenium adsorption, preferably, the preparation of the aerogel is carried out in an argon atmosphere, and the drying is carried out in a condensation dryer.
In the preparation method of the two-dimensional material composite aerogel for rhenium adsorption, preferably, the freeze-drying temperature is-70 to-60 ℃, and the freeze-drying time is 48 to 72 hours.
In the preparation method of the rhenium adsorption two-dimensional material composite aerogel, preferably, in the aerogel preparation step, PDDA (M)w100000-: 1: 1.1-1.2.
The prepared two-dimensional material composite aerogel for rhenium adsorption is a composite material, has the advantages of large specific surface area, rich active sites, high ion exchange capacity, controllable interlamellar spacing, good hydrophilicity and the like, overcomes various defects of liquid-liquid extraction separation of rhenium in a rhenium adsorption enrichment method when being used for adsorbing rhenium metal elements, and has the advantages of high selectivity, high yield and small using amount, and the aerogel can be recycled and recovered, thereby reducing the environmental pollution and lowering the rhenium recovery cost.
Detailed Description
In order to better understand the present invention, the following examples are further illustrative, and it should be understood that the following experiments are intended to better illustrate the present invention, but not to limit the scope of the present invention.
Example 1:
a rhenium adsorption two-dimensional material composite aerogel a is prepared by the following steps:
1) preparing a two-dimensional material: adding LiF into 7.5M hydrochloric acid, stirring until the solution is transparent, and adding Ti with the molar ratio of 1:1 to the LiF2Heating the mixed solution to 35 deg.C, stirring, and reacting for 48 hr; washing the product with deionized water, and centrifuging at 3000rpm for 5 min; repeating the washing and centrifuging cycle for 3 times to obtain stable deep red supernatant; adding deionized water into the supernatant, shaking, centrifuging at 2000rpm for 25min, and collecting the liquid phase to obtain a nanosheet TCNS colloidal solution;
2) preparing aerogel: with vigorous stirring, 2 wt% of PDDA (M)w100000-; after the dropwise addition, the mixture was further stirred under argon for 2 hr; centrifuging at 10000rpm for 5min, and washing the obtained precipitate with deionized water; repeating the centrifuging and deionized water washing operations 3 times to remove excess PDDA; and freeze-drying the washed product at-60 deg.C for 48hr to obtain black aerogel cake TCNS-P, i.e. rhenium adsorption two-dimensional material composite aerogel a, and detecting to obtain product with average pore size of 14.11 nm.
And (3) detecting the rhenium adsorption performance:
loading the two-dimensional material composite aerogel a prepared in the example 1 into an ion exchange column, adsorbing and treating a rhenium-containing material molybdenite oxidation leachate, wherein the component of the leachate is low-grade ammonium rhenate, feeding the leachate into the ion exchange column, adsorbing the ammonium rhenate on the two-dimensional material composite aerogel a, desorbing by using ammonia water after adsorption is finished, and concentrating to obtain an ammonium rhenate concentrated solution; evaporating and concentrating at 90 ℃, standing and crystallizing at 60 ℃, recrystallizing and purifying to obtain an ammonium rhenate product, and testing the adsorption rate and the product purity. Experiment results show that the adsorption rate of the ammonium rhenate on the two-dimensional material composite aerogel a reaches 99.1%, and the purity of the ammonium rhenate can reach 99.94%.
After the composite aerogel a is adsorbed and used, the recovered two-dimensional material composite aerogel a is washed by deionized water and is used as an adsorbent for rhenium adsorption again, and the rhenium adsorption rate is almost unchanged after 10 times of circulation in a circulation experiment.
Example 2:
a rhenium adsorption two-dimensional material composite aerogel b is prepared by the following steps:
1) preparing a two-dimensional material: adding LiF into 8.0M hydrochloric acid, stirring until the solution is transparent, adding Ti with the molar ratio of the Ti to the LiF being 1:1.12Heating the mixed solution to 40 deg.C, stirring, and reacting for 60 hr; washing the product with deionized water, and centrifuging at 4000rpm for 10 min; repeating the washing and centrifuging cycle for 4 times to obtain stable deep red supernatant; adding deionized water into the supernatant, shaking, centrifuging at 2500rpm for 30min, and collecting the liquid phase to obtain a nanosheet TCNS colloidal solution;
2) preparing aerogel: 3 wt% of PDDA (M) was added with vigorous stirringw100000-; after the dropwise addition, the mixture was further stirred under argon for 3 hr; centrifuging at 15000rpm for 10min, and washing the obtained precipitate with deionized water; repeating the centrifugation and deionized water washing operations 4 times to remove excess PDDA; and freeze-drying the washed product at-70 deg.C for 72hr to obtain black aerogel cake TCNS-P (rhenium adsorption two-dimensional material composite aerogel b), and detecting to obtain product with average pore size of 14.14 nm.
And (3) detecting the rhenium adsorption performance:
loading the two-dimensional material composite aerogel b prepared in the embodiment 2 into an ion exchange column, adsorbing molybdenite roasting flue gas eluent, carrying out column-passing adsorption on rhenium-containing materials, and desorbing ammonia water after adsorption to obtain an ammonium rhenate concentrated solution; evaporating and concentrating at 95 ℃, standing and crystallizing at 60 ℃, and recrystallizing and purifying to obtain an ammonium rhenate product. Experiment test results show that the adsorption rate of the ammonium rhenate on the two-dimensional material composite aerogel b can reach 98.7%, and the purity of the ammonium rhenate can reach 99.90%.
Example 3:
a rhenium adsorption two-dimensional material composite aerogel c is prepared by the following steps:
1) preparing a two-dimensional material: adding LiF into 8.5M hydrochloric acid, stirring until the solution is transparent, and adding Ti with the molar ratio of 1:1 to the LiF2Heating the mixed solution to 45 deg.C, stirring, and reacting for 72 hr; washing the product with deionized water, and centrifuging at 3000rpm for 10 min; the washing and centrifugation cycles were repeated 3 times to obtain stabilizationThe deep red supernatant of (a); adding deionized water into the supernatant, shaking, centrifuging at 2500rpm for 35min, and collecting the liquid phase to obtain a nanosheet TCNS colloidal solution;
2) preparing aerogel: 4 wt% of PDDA (M) are added with vigorous stirringw100000-; after the dropwise addition, the mixture was further stirred under argon for 3 hr; centrifuging at 10000rpm for 10min, and washing the obtained precipitate with deionized water; repeating the centrifuging and deionized water washing operations 3 times to remove excess PDDA; and freeze-drying the washed product at-60 deg.C for 72hr to obtain black aerogel cake TCNS-P (rhenium adsorption two-dimensional material composite aerogel c), and detecting to obtain product with average pore size of 14.41 nm.
Rhenium adsorption experiments:
loading the two-dimensional material composite aerogel c prepared in the example 3 into an ion exchange column, treating molybdenite roasting smoke dust leachate, carrying out column adsorption on rhenium-containing materials, desorbing after adsorption is finished, wherein a desorbent is ammonia water, and obtaining an ammonium rhenate concentrated solution; evaporating and concentrating at 95 ℃, standing and crystallizing at 55 ℃, and recrystallizing and purifying to obtain the ammonium rhenate product. Experiment test results show that the adsorption rate of the ammonium rhenate on the two-dimensional material composite aerogel c can reach over 99.0%, and the purity of the ammonium rhenate can reach 98.9%.
The present invention is not described in detail in the prior art.
Claims (7)
1. A preparation method of a two-dimensional material composite aerogel for rhenium adsorption is characterized by comprising the following steps: the method comprises the following steps:
1) preparing a two-dimensional material: adding LiF into hydrochloric acid, stirring until the solution is transparent, and adding Ti2Heating the mixed solution of AlC powder, stirring and reacting at a constant temperature; washing the product with deionized water, and centrifuging at 3000-; repeating the washing and centrifugation cycles until a stable deep red supernatant is obtained; adding deionized water into the supernatant, shaking, centrifuging at 2000-;
2) preparing aerogel: PDDA (M) was added with vigorous stirringw100000-S in colloidal solution; after the dropwise addition, further stirring the mixture for 2-3hr under inert atmosphere; centrifuging at 10000-; repeating the operations of centrifugation and deionized water washing for 3-4 times; and (3) freeze-drying the washing product to obtain a black aerogel cake TCNS-P, namely the two-dimensional material composite aerogel for absorbing rhenium.
2. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: in the preparation step of the two-dimensional material, the concentration of hydrochloric acid is 7.5-8.5M, the reaction temperature is 35-45 ℃, and the reaction time is 48-72 hr.
3. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: in the step of preparing the two-dimensional material, LiF and Ti2The molar ratio of AlC is 1: 1.0-1.1.
4. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: in the aerogel preparation step, PDDA (M)w100000-.
5. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: aerogel preparation is carried out under argon atmosphere, and drying is carried out in a condensation dryer.
6. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: the freeze drying temperature is-70-60 deg.C, and the freeze drying time is 48-72 hr.
7. The method for preparing a rhenium-adsorbing two-dimensional material composite aerogel as claimed in claim 1, wherein: in the aerogel preparation step, PDDA (M)w100000-: 1: 1.1-1.2.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328890A (en) * | 2016-08-26 | 2017-01-11 | 浙江工业大学 | Carbon-pillared MXene composite material and application thereof |
| CN109706507A (en) * | 2019-01-16 | 2019-05-03 | 华南理工大学 | A kind of two-dimentional MXene film and preparation method thereof with vertical channel structure |
| US20200239363A1 (en) * | 2016-12-16 | 2020-07-30 | Imperial College Of Science, Technology And Medicine | Composite material |
| CN113451590A (en) * | 2021-06-29 | 2021-09-28 | 合肥工业大学 | Preparation method of MXene-based catalyst with ion/electron double transmission |
| WO2021196864A1 (en) * | 2020-04-02 | 2021-10-07 | 北京航空航天大学 | Mxene composite gel material, preparation method and use |
| CN113624735A (en) * | 2021-06-30 | 2021-11-09 | 中山大学 | Magnetic nano composite material, preparation method thereof and application of magnetic nano composite material in SERS detection |
-
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- 2021-12-31 CN CN202111649147.XA patent/CN114259998A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328890A (en) * | 2016-08-26 | 2017-01-11 | 浙江工业大学 | Carbon-pillared MXene composite material and application thereof |
| US20200239363A1 (en) * | 2016-12-16 | 2020-07-30 | Imperial College Of Science, Technology And Medicine | Composite material |
| CN109706507A (en) * | 2019-01-16 | 2019-05-03 | 华南理工大学 | A kind of two-dimentional MXene film and preparation method thereof with vertical channel structure |
| WO2021196864A1 (en) * | 2020-04-02 | 2021-10-07 | 北京航空航天大学 | Mxene composite gel material, preparation method and use |
| CN113451590A (en) * | 2021-06-29 | 2021-09-28 | 合肥工业大学 | Preparation method of MXene-based catalyst with ion/electron double transmission |
| CN113624735A (en) * | 2021-06-30 | 2021-11-09 | 中山大学 | Magnetic nano composite material, preparation method thereof and application of magnetic nano composite material in SERS detection |
Non-Patent Citations (2)
| Title |
|---|
| CHENGCHENG XING ET AL.，: "MXene@Poly(diallyldimethylammonium chloride) Decorated Carbon Cloth for Highly Electrochemically Active Biofilms in Microbial Fuel Cells", 《CHEMELECTROCHEM》 * |
| 宋环: "二维过渡金属碳化物对Eu（Ⅲ）和Re（Ⅶ）吸附行为研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 1, pages 014 - 1262 * |
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