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Alicyclic crown ether bonding type silicon resin and preparation method thereof

A silicone resin and cycloaliphatic technology, which is applied in the field of preparation of metal ion extraction and adsorption materials, can solve the problems of easy loss in the extraction process, poor stability, poor repeatability, and increased cost, and achieve stability and reusability. Large extraction adsorption capacity, avoiding the effect of loss

Active Publication Date: 2012-07-18
四川华冠众邦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide an alicyclic crown ether bonded silicone resin, which solves the problem of weak interaction between the alicyclic crown ether and the silicone resin matrix in the existing similar technology, and it is easy to lose during the extraction process, thereby causing stability. , poor repeatability, and increased cost

Method used

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  • Alicyclic crown ether bonding type silicon resin and preparation method thereof
  • Alicyclic crown ether bonding type silicon resin and preparation method thereof
  • Alicyclic crown ether bonding type silicon resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: Preparation of silicone resin precursor containing 3-chloropropyl

[0035]Take 0.05mol tetraethoxysilane and 0.05mol 3-chloropropyltriethoxysilane and dissolve them in 0.5mol ethanol. 0.35 mol of deionized water was slowly added dropwise, and dibutyltin dilaurate was added as a catalyst accounting for 1 mol% of the total amount of silane monomers, stirred and mixed evenly, and left to stand at room temperature for 3 days. Then place it in a vacuum oven at 120° C. for 8 hours. The obtained resin is ground to obtain micron-sized particles, that is, the precursor of silicone resin containing 3-chloropropyl group.

Embodiment 2

[0036] Embodiment 2: Preparation of silicone resin precursor containing 3-bromopropyl

[0037] Mix and dissolve 0.3 mol tetramethoxysilane and 0.1 mol 3-bromopropyltrimethoxysilane in 2.0 mol ethanol. Slowly add 1.5 mol of deionized water dropwise while stirring. The catalyst is triethylamine, and the added amount accounts for 3 mol% of the total amount of silane monomers. After mixing evenly, it was left to stand at 30°C for 2 days. Then place it in a vacuum oven at 100°C for 5 hours. Take out and grind to obtain micron-sized resin particles, that is, the silicone resin precursor containing 3-bromopropyl group.

Embodiment 3

[0038] Embodiment 3: Preparation of silicone resin precursor containing 3-iodopropyl

[0039] Weigh 0.1mol methyltriethoxysilane, 0.4mol 3-iodopropyltriethoxysilane, add 2.5mol ethanol, and stir evenly. Keep stirring and slowly add 1.6 mol deionized water dropwise, and add ammonia water accounting for 5 mol% of the total amount of silane monomers as a catalyst, mix well, and let stand at 40° C. for 3 days. It was further treated in a vacuum oven at 150°C for 4 hours, and the obtained resin was ground into fine particles, that is, a silicone resin precursor containing 3-iodopropyl group.

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Abstract

The invention discloses alicyclic crown ether bonding type silicon resin and a preparation method thereof in the technical field of the preparation of metal ion extraction and adsorption material. The alicyclic crown ether bonding type silicon resin comprises dicyclohexyl crown ether bonding silicon resin with a structure shown in a general formula I and cyclohexyl crown ether bonding silicon resin with a structure shown in a general formula II. The resin synthesis method comprises the steps that a silicon resin precursor containing a halogenated alkyl active group is firstly prepared; and then an alicyclic crown ether extraction agent is fixed on resin material in a chemical bonding manner on the basis of a nucleophilic substitution reaction of an amino-substituted alicyclic crown ether compound and halogenated alkyl. The alicyclic crown ether bonding type silicon resin disclosed by the invention can prevent the crown ether extraction agent from being lost in the metal ion extractionand separation process and guarantees the stability and the reusability of the extraction performance; and the content of the alicyclic crown ether extraction agent in the silicon resin is high, so that the enhancing of the extraction and adsorption quantity of metal ion is facilitated.

Description

technical field [0001] The invention belongs to the technical field of preparation of metal ion extraction adsorption materials, and in particular relates to an alicyclic crown ether bonded silicone resin and a preparation method thereof. Background technique [0002] The extraction and separation of metal ions by using the specific complexation ability of crown ether compounds to metal ions in solution has always attracted much attention. Crown ethers were first invented and reported by Dr. Pedersen of DuPont, and their synthesis is generally based on typical Williamson ether synthesis reactions. The special property of crown ether is that it has a strong coordination ability for alkali metal and alkaline earth metal cations. The principle is to form a stable complex with the corresponding metal ions through the hydrophobic outer skeleton and hydrophilic inner cavity in the crown ether structure. structure. The stability of complexes formed by crown ether compounds and me...

Claims

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Application Information

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IPC IPC(8): C08G77/388C08G77/24B01J20/30B01J20/26
Inventor 叶钢白飞飞韦继超王建晨陈靖
Owner 四川华冠众邦科技有限公司
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