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Novel class of calixarene crown ether bond-type silicon-based adsorption materials and preparation method thereof

An adsorption material, hydrocarbon crown ether technology, applied in the direction of selective adsorption, chemical instruments and methods, other chemical processes, etc., can solve the problems of reducing the stability and reuse efficiency of adsorption materials, loss and decomposition, weak binding force, etc., to achieve excellent Thermal and chemical stability, avoidance of bleed, improved force effect

Inactive Publication Date: 2013-04-24
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0008] However, there are still some shortcomings in the existing research
Extractants that are selective to cesium ions are all loaded on inert substrates through physical effects such as adsorption and envelopment, and the binding force between the two is weak, which will lead to the loss of a large number of extractant molecules in strong acidic and radioactive environments Or decompose, greatly reducing the stability and reuse efficiency of adsorption materials

Method used

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  • Novel class of calixarene crown ether bond-type silicon-based adsorption materials and preparation method thereof
  • Novel class of calixarene crown ether bond-type silicon-based adsorption materials and preparation method thereof
  • Novel class of calixarene crown ether bond-type silicon-based adsorption materials and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0046] Embodiment 1: the synthesis of Si-3-Calixcrown

[0047] Weigh 3.5 g of diamino-substituted bis(2-propoxy)calix[4]arene-crown-6 and dissolve it in 100 mL of tetrahydrofuran (THF), add 8.7 g of 3-chloropropyl-containing silicon-based precursor , and added 14.3 g K 2 CO 3 and 6.1 g KI. Keep stirring and under nitrogen atmosphere, reflux at 85°C for 12 h. The solid particles were separated by filtration, and washed repeatedly with deionized water and ethanol to remove salt ions. Recycling of unreacted bonded diaminobis(2-propoxy)calix[4]arene-crown-6 monomer. The obtained adsorption material particles are dried under vacuum condition, and the solvent is removed to obtain the final product.

[0048] The infrared spectrum of the prepared calixarene crown ether bonded silicon-based material is shown in figure 1 shown. By comparison, it can be clearly seen that in the spectrum of the bonding material, the wave numbers are 3426, 3349 cm -1 There are obvious amine-based a...

Embodiment 2

[0049] Embodiment 2: the synthesis of Si-5-Calixcrown

[0050] Dissolve 5.7 g of diaminobis(2-propoxy)calix[4]arene-crown-6 in 80 mL of N,N-dimethylformamide (DMF), add 12.5 g of 5-bromopentyl Silicone precursors. The catalysts are NaOH and NaI, and the addition amounts are NaOH8.5 g and NaI6.4 g, respectively. Under the protection of nitrogen gas, the reaction was stirred and refluxed at 100°C for 10 h. After the reaction, the resin particles were separated by filtration. Unreacted bonded diaminobis(2-propoxy)calix[4]arene-crown- enters the filtrate, which can be recycled. The solid resin particles are repeatedly washed with deionized water and ethanol to completely elute the corresponding salt ions and entrained crown ether monomers, and then vacuum-dried to remove the solvent to obtain the final product.

Embodiment 3

[0051] Embodiment 3: the synthesis of Si-7-Calixcrown

[0052] Weigh 9.6 g of diaminobis(2-propoxy)calix[4]arene-crown-6 and dissolve it in 150 mL of N,N-dimethylacetamide, add 20.3 g of silicon containing 7-iodoheptyl base precursor, and added 4.8 g NaH. Keep stirring and under nitrogen atmosphere, react at 75°C for 8 h. The resin particles were separated by filtration, and washed repeatedly with deionized water, ethanol, and hot acetone to remove salt ions. Recycling of unreacted bonded diaminobis(2-propoxy)calix[4]arene-crown-6 monomer. The obtained solid particles are dried under vacuum conditions, and the solvent is removed to obtain the final product.

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Abstract

The present invention discloses a novel class of calixarene crown ether bond-type silicon-based adsorption materials and a preparation method thereof, belonging to the technical field of metal ion adsorption material preparation. The adsorbent materials have the structure shown in the formula below: wherein, R is H or; and X = 2-12. During the preparation of the adsorbent materials, firstly modifying di(2-propoxy)calix [4] arene-crown-6 to bring reactive amino group to the molecular structure; then a preparing silicon-based precursor containing haloalkyl; and finally reacting amino-substituted di(2-propoxy)calix [4] arene-crown-6 with the silicon-based precursor containing haloalkyl, so that the calixarene crown ether groups are bonded on the silicon carrier to get a novel class of calixarene crown ether bond-type silicon-based adsorption materials. The method provided by the invention is simple in operation; and the obtained adsorption materials have excellent thermal stability and chemical stability, high reusability, and large adsorption capacity for cesium ions.

Description

technical field [0001] The invention belongs to the technical field of preparation of metal ion adsorption materials, and in particular relates to a novel calixarene crown ether bonded silicon-based adsorption material and a preparation method thereof. Background technique [0002] Last year, the Fukushima Nuclear Power Plant leakage accident triggered by the "3.11" earthquake in Japan caused serious radioactive cesium pollution. The content of cesium-137 in the seawater and soil around Fukushima seriously exceeded the standard. Cesium-137 is one of the long-lived splinter elements produced in the process of nuclear fuel fission. It has strong radioactivity and high heat release capacity, and mainly exists in the high-level waste liquid produced by the reprocessing of spent fuel. Separating elements such as cesium-137 and strontium-90 and treating them separately will help convert high-level waste liquid into medium-low level waste liquid, which can greatly reduce the volume...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D15/08
Inventor 叶钢冷雨潇白飞飞韦继超王建晨陈靖
Owner TSINGHUA UNIV
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