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Preparation method of silica gel loaded polyhydroxyl chelating resin for highly effective boron removal

A technology of chelating resin and polyhydroxyl, which is applied in the field of preparation of chelating resin, can solve the problems of complex synthesis process, low adsorption capacity and high cost, and achieve the effects of large adsorption capacity, improved adsorption capacity and good mechanical strength

Inactive Publication Date: 2012-04-11
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this synthesis method, the generation of modified silane coupling agent can effectively reduce the alkalinity of meglumine in the reaction system, avoid the dissolution of silica gel in the modification process, and effectively improve the synthesis efficiency of the resin, but this method synthesizes The particle size distribution of the resin is too wide, the adsorption capacity is low, the cost is expensive and the synthesis process is complicated, it is difficult to effectively promote in practical applications (O.Kaftan, M.Acikel, A.E.Eroglu, T.Shahwan, L.Artok, C.Ni , Synthesis, characterization and application of a novel sorbent, glucamine-modified MCM-41, for the removal / preconcentration of boron from waters, Anal.Chim.Acta 2005, 547:31~41; B.Tural, Separation and preconcentration of boron with a glucamine modified novel magnetic sorbent. Clean-Soil, Air, Water 2010, 38: 321~327; H.N.Liu, X.S.Ye, Q.Li, T.Kim, B.J.Qing, M.Guo, F Ge, Z.J.Wu, K. Lee, Boron absorption using a new boron-selective hybrid gel and the commercial resin D564. Colloids and Surfaces A: Physicochemical and Engineering Aspects 2009, 341: 118~126.)

Method used

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  • Preparation method of silica gel loaded polyhydroxyl chelating resin for highly effective boron removal
  • Preparation method of silica gel loaded polyhydroxyl chelating resin for highly effective boron removal

Examples

Experimental program
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Embodiment 1

[0027] Embodiment 1 adopts different inert organic solvents to prepare meglumine modified silane coupling agent

[0028] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0029] (2) Add 20g of meglumine and 200ml of inert organic solvent to a 500ml three-necked flask, mechanically stir, and heat in an oil bath to raise the temperature of the reaction system to 50-100°C; 40ml of inert organic solvent and 30ml of 3-(2,3-cyclo Oxypropoxy)propyltrimethoxysilane was mixed evenly and then dropped into the three-neck flask dropwise. During the whole reaction process, the system temperature was kept at 80° C., and the nitrogen atmosphere was refluxed for 24 hou...

Embodiment 2

[0033] Example 2 Using different inert organic solvents to prepare silica gel-loaded polyhydroxyl efficient boron-removing chelating resins

[0034] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0035] (2) Take 20g meglumine and 200ml N,N-dimethylformamide and add them to a 500ml three-necked flask, stir mechanically, heat the oil bath to raise the temperature of the reaction system to 80°C; 40ml N,N-dimethylformamide and 30ml of 3-(2,3-glycidoxy)propyltrimethoxysilane was mixed evenly and then dropped into the three-necked bottle drop by drop. During the whole reaction process, the system temperature was kept at 80°C, and the nitrogen atmosphere wa...

Embodiment 3

[0039] Example 3 Using different silane coupling agents to prepare silica gel-loaded polyhydroxyl efficient boron-removing chelating resins

[0040] (1) Take 30g of chromatographically packed silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0041] (2) Take 20g meglumine and 200ml N,N-dimethylformamide and add them to a 500ml three-necked flask, stir mechanically, heat the oil bath to raise the temperature of the reaction system to 80°C; 40ml N,N-dimethylformamide and 30ml of silane coupling agent was mixed evenly and then dropped into the three-neck bottle drop by drop. During the whole reaction process, the temperature of the system was kept at 80°C, and the nitrogen atmosphere was refluxed fo...

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Abstract

The invention relates to a preparation method of chelating resin for highly effective boron absorption, especially a preparation method of silica gel loaded polyhydroxyl chelating resin for highly effective boron removal. The method comprises reacting meglumine and silane coupling agent in inert organic solvent, generating meglumine modified silane coupling agent, making the meglumine modified silane coupling agent react with activated silica gel, and finally generating a silica gel loaded polyhydroxyl chelating resin for highly effective boron removal. Compared with the conventional macromolecule-based boron-removing chelating resin, the invention has simple and economical method, overcomes the detects in the present synthesis flow that the silica gel is dissolved for alkalinity of the reaction system is too high (pH more than 11) when surface modified halogen or silica gel of epoxide group reacts with meglumine to synthesize the silica gel loaded polyhydroxyl boron-removing chelating resin, or that the silica gel loaded polyhydroxyl boron-removing chelating resin cannot be synthesized for the nucleophilic substitution of halogen or epoxide group with meglumine cannot be carried out effectively when alkalinity of the reaction system is too low (pH less than 10).

Description

Technical field: [0001] The invention relates to a preparation method of a chelating resin with high-efficiency adsorption performance on boron, in particular to a preparation method of a silica gel-loaded polyhydroxy efficient boron-removing chelating resin. Background technique: [0002] my country is rich in boron resources, and boron reserves rank fifth in the world, but there are many lean ores and few rich ores. With decades of mining, high-grade solid boron ore resources are close to exhaustion. Therefore, from the salt lake brine rich in boron resources Boron extraction has become the main way to obtain boron resources in recent years. The methods for extracting boron from salt lake brine mainly include: acidification precipitation method, flotation method, chelation adsorption method, solvent extraction method, etc. Among them, chelation adsorption method is suitable for treating brine with low boron concentration, and it has strong selectivity, It has broad applica...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/30
Inventor 胡慧萍徐璐陈启元刘云清白蓝
Owner CENT SOUTH UNIV
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