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Mesoporous materials modified with amine groups and their application in the separation of molybdenum and rhenium

A technology of mesoporous material and amine-based function, applied in the field of mesoporous material preparation and effective extraction of scattered metals, can solve the problems of unsatisfactory separation effect of molybdenum and rhenium, co-adsorption and co-analysis of molybdenum and rhenium, and difficulty in extraction and separation. , to achieve the effect of abundant raw materials, reduced processing costs and low costs

Active Publication Date: 2017-01-11
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Since the properties of molybdenum and rhenium are very similar, and rhenium itself has no independent deposit, it can only be associated with molybdenite and other deposits, so it is not easy to separate molybdenum and rhenium completely simply and effectively, especially When a large amount of molybdenum and a small amount of rhenium coexist, molybdenum exists in various and complex forms, making extraction and separation even more difficult, and there is a problem of co-adsorption and co-analysis of molybdenum and rhenium during separation
At present, the methods for extracting molybdenum mainly include extraction method, liquid membrane method, co-crystallization method, ion exchange method, precipitation method, activated carbon adsorption method and foam flotation. The separation methods for rhenium mainly include extraction method, ion exchange method and liquid membrane method. And activated carbon adsorption method, after continuous improvement, there are still problems such as lengthy process, unsatisfactory separation effect of molybdenum and rhenium, and the recovery rate of rhenium needs to be further improved.

Method used

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  • Mesoporous materials modified with amine groups and their application in the separation of molybdenum and rhenium
  • Mesoporous materials modified with amine groups and their application in the separation of molybdenum and rhenium
  • Mesoporous materials modified with amine groups and their application in the separation of molybdenum and rhenium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]Example 1 Amino functionalized modified mesoporous material B7SS-5-3h-5.5@0.2NH 2

[0034] First, mix 7g of mesitylene with P123 solution (dissolve 4.0g of P123 in 120mL of deionized water, and add 20mL of HCl) to obtain a mixed solution A, and the first part of 5g of Na 2 SiO 3 Dissolve in deionized water of equal mass, add to mixed solution A, and stir at 40°C to obtain mixed solution B. After reacting for 3h, the second part of 5.5g Na 2 SiO 3 Dissolve it in deionized water of equal mass, then add it dropwise to the mixed solution B, stir at 40°C for 6h, age at 100°C for 24h, filter with suction, wash the precipitate, and dry. The dried product was placed in a muffle furnace, heated to 550°C at a rate of 1-2°C / min, and roasted for 4 hours to obtain the product SBA-15, named B7SS-5-3h-5.5, with a yield of 21%.

[0035] Put the prepared 2.21g (0.0368mol) of SBA-15 in a three-necked flask, add 80mL of ethanol solution, add 1.63g (0.0074mol) of APTES under nitrogen p...

Embodiment 2

[0037] Example 2 Amino functionalized modified mesoporous material SS-5-3hB7-5.5@0.2NH 2

[0038] The first part of 5g Na 2 SiO 3 Dissolve in deionized water of equal mass, then add dropwise into P123 solution (4.0g P123 dissolved in 120mL deionized water, and add 20mL HCl), stir at 40°C to obtain mixed solution C. After reacting for 3 hours, first add 7g of mesitylene into the above mixed solution C, stir to obtain mixed solution D, and then add 5.5g of the second part of Na 2 SiO 3 Dissolve it in deionized water of equal mass, then add it dropwise to the mixed solution D, stir at 40°C for 6h, age at 100°C for 24h, filter with suction, wash the precipitate, and dry. The dried product was put into a muffle furnace, heated at a rate of 1-2°C / min to 550°C and calcined for 4 hours to obtain SBA-15, named SS-5-3hB7-5.5, with a yield of 20%.

[0039] Put the prepared 2.1g (0.035mol) of SBA-15 in a three-necked flask, add 80mL of ethanol solution, add 1.55g (0.007mol) of APTES ...

Embodiment 3

[0044] Example 3 Effect of Amino-functionalized Modified Mesoporous Materials on the Molybdenum-Rhenium Separation Effect at Different Acidity and Molar Ratio

[0045] Method: Take 5 mL of each solution containing Mo(VI) 20ppm and Re(VII) 20ppm ions, adjust the acidity of the solution to pH=10, pH=8, pH=6, pH=3, pH=1, 1mol L -1 , 3mol L -1 ; Regulate the molar ratio of SBA-15 and APTES to be 1:0.1, 1:0.2, 1:0.3, 1:0.4 respectively. Then add 10 mg of amine functionalized modified mesoporous material B7SS-5-3h-5.5@nNH 2 or SS-5-3hB7-5.5@nNH 2 , oscillating adsorption for 24 hours, the result is as follows figure 1 with figure 2 shown.

[0046] Depend on figure 1 with figure 2 It can be seen that after modification, the adsorption effect on molybdenum is better, up to 100%, and there is basically no adsorption on rhenium, so the effect of separating molybdenum and rhenium can be effectively achieved. B7SS-5-3h-5.5@0.2NH 2 and SS5-3hB7-5.5@0.2NH 2 The maximum adsorptio...

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Abstract

The invention relates to an amine-containing functional mesoporous material and application thereof to separation of rhenium and molybdenum. According to the technical scheme, the material is prepared by the following steps: dissolving a first part of Na2SiO3 in deionized water, adding to a mixing solution of mesitylene and P123, and stirring at 40 DEG C; reacting for a certain period of time, dissolving a second part of Na2SiO3 in deionized water, adding to the mixing solution, stirring at 40 DEG C for 6 hours, aging at 100 DEG C for 24 hours, performing suction filtration, washing and drying to obtain a product; roasting the dried product in a muffle furnace at 550 DEG C for 4 hours to obtain an SBA-15 product; and placing the SBA-15 product in a three-neck bottle, adding 80mL of ethanol solution, adding certain amount of APTES under protection of nitrogen, stirring for 30 minutes, slowly dropwise adding 20mL of H2O, stirring for 30 minutes, performing suction filtration, and drying at 110 DEG C for 24 hours to obtain the final product. The method is simple, and is low in cost and high in adsorption amount, and rhenium and molybdenum separation selectivity is high.

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous materials and effective extraction of scattered metals, in particular to a mesoporous material modified with amine groups to selectively and effectively adsorb molybdenum ions from a solution containing other heavy metal ions to achieve efficient separation of molybdenum and rhenium the goal of. Background technique [0002] Due to the special physical and chemical properties of scattered metals (gallium, indium, thallium, germanium, selenium, tellurium, rhenium) and their compounds, more and more researchers pay attention to them. Especially molybdenum (Mo), which is a widely used element in scattered metals, and metal Mo and Mo alloys are excellent engineering materials. Molybdenum has excellent properties such as high melting point and high boiling point, good electrical conductivity, thermal conductivity, and wear resistance. Molybdenum is widely used in biopharmaceuticals,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/08
CPCB01D15/08B01J20/10B01J20/22B01J20/28054
Inventor 单炜军张庆熊英王伟娄振宁茹红强
Owner LIAONING UNIVERSITY
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