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Preparation method of inorganic ion exchange material for stationary phase in solid phase extraction

An inorganic ion exchange and stationary phase technology, applied in separation methods, inorganic chemistry, chemical instruments and methods, etc., can solve problems such as limited production conditions for large-scale use, poor mechanical strength and hydraulic properties, and inability to meet industrial applications. , to achieve the effect of good hydraulic performance and mechanical strength, high extraction capacity and partition coefficient, and low cost

Inactive Publication Date: 2016-05-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most ion exchange materials with high extraction capacity and specific selectivity, such as heteropolyacid salts, polyvalent metal phosphates, ferrous and ferricyanide, etc., most of them suffer from poor mechanical strength and hydraulic properties. As a result, industrial applications such as column packing operation and extraction cannot be met
In recent years, ion-exchange materials have been loaded into porous silica channels under vacuum conditions to improve their mechanical strength by using the in-pore crystallization method (Wang Qilong et al. Synthesis of silicon-based ammonium phosphomolybdate adsorbent and its adsorption to Cs [J], Nuclear Chemistry and Radiation Chemistry, 2014,36(4):210-215.), there are also composite ion exchange materials using sol-gel method, after high temperature and high pressure sintering, the material can meet the requirements of column operation, but these Factors such as vacuum, high temperature and high pressure required by the technology and high cost limit the large-scale use of its production conditions

Method used

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  • Preparation method of inorganic ion exchange material for stationary phase in solid phase extraction
  • Preparation method of inorganic ion exchange material for stationary phase in solid phase extraction
  • Preparation method of inorganic ion exchange material for stationary phase in solid phase extraction

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Embodiment 1

[0018] Embodiment 1: a kind of preparation method of inorganic ion exchange material used for stationary phase in solid phase extraction, comprises the following steps:

[0019] A. Synthesis of matrix agent: use ethanol as solvent, add tetraethyl orthosilicate and polyvinyl alcohol 1788 accounting for 2-5% of water solvent mass percentage according to a certain volume ratio, the mass ratio is about 10:7.2:10g, Under normal temperature and pressure conditions, stir evenly, at 5-7mol L -1 Hydrochloric acid (volume: 0.1 ~ 0.4mL) solution to react, the reaction time is until the solution system is transparent, so that they are mixed together;

[0020] B, the synthesis of extractant: in water solvent, add potassium pyrophosphate (K 4 P 2 o 7 2H 2 O), sodium molybdate (Na 2 MoO 4 2H 2 O), zirconium oxychloride (ZrOCl 2 ·8H 2 O), where Na 2 MoO 4 2H 2 O use 0.93g, use 4 ~ 7mol L -1 Nitric acid (volume: 0.3 ~ 0.8mL) solution was acidified, mixed evenly, a chemical reactio...

Embodiment 2

[0024] Embodiment 2: a kind of preparation method of inorganic ion exchange material used for stationary phase in solid phase extraction, comprises the following steps:

[0025] A. Synthesis of matrix agent: use water as solvent, add silica gel and polyethylene glycol 400 with a mass percentage of 3-5% of water solvent according to a certain volume ratio, the mass ratio is about 10:8:10g, normal temperature and pressure Stir evenly under the condition of 5~7mol L -1 Hydrochloric acid (volume: 0.1 ~ 0.4mL) solution to react, the reaction time is until the solution system is transparent, so that they are mixed together;

[0026] B. Synthesis of extractant: accurately weigh zirconium oxychloride (ZrOCl) according to the stoichiometric ratio 2 ·8H 2 O) 1.61g in a beaker, then add 5mL of water to ZrOCl 2 ·8H 2 O dissolves completely. Immediately, pipette gun to pipette 85% phosphoric acid (volume: 0.5mL), slowly add it dropwise into the beaker, keep stirring at room temperatur...

Embodiment 3

[0030] Embodiment 3: a kind of preparation method of inorganic ion exchange material used for stationary phase in solid phase extraction, comprises the following steps:

[0031] A. Synthesis of matrix agent: take methanol as solvent, add tetraethyl orthosilicate and polyethylene glycol 2000 accounting for 3-5% by mass of water solvent in a certain volume ratio, and the mass ratio is about 10:10:10g , under the condition of normal temperature and pressure, stir evenly, in nitric acid 5 ~ 8mol L -1 Nitric acid (volume: 0.1 ~ 0.4mL) solution to react, the reaction time is until the solution system is transparent, so that they are mixed together;

[0032] B. Synthesis of extractant: Accurately weigh ferric chloride (FeCl 3 ) and potassium ferrocyanide (K 4 [Fe(CN) 6 ]) in a beaker, in which 0.46gFeCl 3 , and then add 10mL of water to dissolve it completely, then add it to the reaction vessel, stir continuously at normal temperature and pressure for 1h to fully react, and gener...

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Abstract

The invention discloses a preparation method of an inorganic ion exchange material for a stationary phase in solid phase extraction. The preparation method includes the steps that a silicon source and a surface alterant are added into a matrix solvent I or II, and the materials are stirred evenly at the normal pressure and temperature and are reacted under the acidic condition to be combined; raw material components with efficient extraction performance on recyclable elements, rare elements and radioactive elements are selected and are synthesized according to a stoichiometric ratio to obtain an extractant; the two mixed systems are mixed evenly, a dispersant is added, and the materials are fused at the normal pressure and the temperature of 50-80 DEG C to generate precipitate jointly; finally, the obtained precipitate is subjected to standing, filtering and washing to obtain a particle material, the particle material is dried to a constant weight, ground and screened, and the inorganic ion exchange material is obtained. The preparation method is simple, fast and low in cost; the extractant can be recycled and has efficient selectivity; the extraction capacity and the distribution coefficient are high; hydraulic performance and mechanical strength are good.

Description

technical field [0001] The invention relates to the preparation of ion exchange materials with high efficiency and selectivity for recyclable, toxic or radioactive elements in the fields of biology, medicine, food, nuclear industry and environment, and specifically relates to the inorganic ion exchange materials used for stationary phases in solid phase extraction. The method of preparation of the material. Background technique [0002] Solid-phase extraction is a technique for sample purification and separation using the distribution of the separated substance between the liquid-solid two phases. This technology can further use ion-exchange materials as fillers to fill the extraction column as a stationary phase, and the separated substances in the sample solution are selectively adsorbed into the stationary phase, so that the separated substances and interfering components can be separated at the same time; The elution of the eluent can separate and enrich the separated s...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/30B01D15/10
CPCB01J20/10B01D15/10
Inventor 李玉香邓浩马雪吴浪黄毅辛利平
Owner SOUTHWEAT UNIV OF SCI & TECH
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