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Preparation method of phenyl boryl modified covalent affine magnetic solid phase extractant

A solid-phase extractant and magnetic technology, applied in chemical instruments and methods, separation methods, solid adsorbent liquid separation, etc., can solve the problems of many reaction steps, low yield, unstable phenylboron group, etc., to simplify the reaction. process, improvement of synthesis conditions, and the effect of simplifying the reaction process

Inactive Publication Date: 2018-05-08
QINGHAI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Phenylboryl-functionalized magnetic solid-phase extraction technology is mostly coated with silicon dioxide with tetraethylorthosilicate as the silicon source outside the magnetic iron ferric oxide core, and then uses Si-OH as the functional group for silane coupling. Wait for the organosilicon reaction to graft the required functional groups to the silicon surface. The disadvantage of the organosilicon reaction is the need to strictly control the anhydrous and oxygen-free conditions
In addition, in the subsequent step of modifying phenylboryl groups, the common method is to use compounds such as aminophenylboronic acid and tetravinylphenylboronic acid as raw materials to react with surface-modified functional groups. On the one hand, this phenylboryl compound is more expensive. On the other hand, in the synthesis process, the phenylboryl group is unstable, and it is often necessary to protect the phenylboryl group when it reacts with organosilicon. Not only the reaction steps are many, but also a little careless operation will lead to low yield.

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  • Preparation method of phenyl boryl modified covalent affine magnetic solid phase extractant

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preparation example Construction

[0016] The present invention provides a technical solution: the present invention provides the following technical solution: a preparation method of a phenylboryl-modified covalent affinity magnetic solid-phase extraction agent, the inner core of which is ferric oxide, and the outer coating is triethoxy base silane, and modify the phenyl boron group on its surface, its synthesis steps and structure are as follows:

[0017]

[0018] Concrete steps of the present invention are:

[0019] A. With ferric oxide as the inner core, add triethoxysilane under acidic conditions, and carry out hydrolysis reaction at 70°C to coat the outer layer of ferric ferric oxide nanoparticles, magnetically separate and discard the reaction solution , to obtain ferric oxide particles coated with triethoxysilane;

[0020] B. Add the iron ferric oxide particles coated with triethoxysilane obtained in the above step A into DMF as the reaction solution, then add sodium carbonate to adjust the reaction...

Embodiment 1

[0023] The preparation of the covalent affinity type magnetic solid-phase extraction agent modified by phenylboryl group comprises the steps:

[0024] (a) Add 1.89g of anhydrous ferric chloride to a 100mL single-necked flask, add 70mL of ethylene glycol, stir for 30min to dissolve, add 4.8g of anhydrous sodium acetate, continue the reaction for 30min, and transfer to a polytetrafluoroethylene reactor After reacting at 200°C for 10h, take it out, cool to room temperature, wash with water and ethanol several times, and dry the ferric oxide spherical particles at 40°C for 24h in vacuum.

[0025] (b) Mix deionized water and ethanol according to the volume ratio of 1:8, adjust the pH to 4.0 with acetic acid, add triethoxysilane with the same volume as deionized dropwise under stirring, and stir at room temperature for 4 hours, make it fully hydrolyzed;

[0026] (c) In a 100ml three-necked flask equipped with a reflux condenser and a thermometer, add the hydrolyzate obtained in (b)...

Embodiment 2

[0032] The covalent affinity magnetic nanoparticles modified by the phenylboryl group of this example are used as a magnetic solid-phase extraction agent to selectively adsorb rare precious metal rubidium ions in aqueous solution. The steps are:

[0033](a) Preparation of stock solution: Accurately weigh 10 mg of rubidium chloride standard substance, dissolve in deionized water and make up to 10 mL.

[0034] (b) Prepare the solution to be tested: accurately pipette 100 μL of the stock solution prepared in step (a), and dilute to 10 mL with deionized water.

[0035] (c) SPE activation step: Accurately weigh 100mg of the prepared magnetic SPE, activate with 5ml of methanol and 3mL of 0.13% acetic acid solution (pH=3) successively, and separate the extraction agent and the solution with an external magnetic field each time , and the supernatant was discarded, and then washed several times with deionized water until the pH of the extractant was approximately neutral.

[0036] (e)...

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Abstract

The invention discloses a preparation method of a phenyl boryl modified covalent affine magnetic solid phase extractant. The method comprises the following steps: using ferroferric oxide as a magneticcore; coating the magnetic core with silicon dioxide by using triethoxysilane as a silicon source; reacting under the condition of sodium carbonate by taking bromobenzyl bromide as a raw material; grafting bromobenzene outside a silicon dioxide coating layer; lastly, preparing the phenyl boryl modified covalent affine magnetic solid phase extractant from biborate serving as a raw material under the catalysis of dichloroferrocene palladium chloride. The covalent affine magnetic solid phase extractant disclosed by the invention belongs to a new generation of magnetic solid phase extractant. Compared with the conventional solid phase extractants, the covalent affine magnetic solid phase extractant has the advantages of easiness and convenience in synthesis, milder synthesis conditions and moderate particle size.

Description

technical field [0001] The invention relates to the technical field of solid-phase extractant preparation, in particular to a preparation method of a phenylboryl-modified covalent affinity magnetic solid-phase extractant. Background technique [0002] Phenylboryl-functionalized magnetic solid-phase extraction technology is mostly coated with silicon dioxide with tetraethylorthosilicate as the silicon source outside the magnetic iron ferric oxide core, and then uses Si-OH as the functional group for silane coupling. Wait for the organosilicon reaction to graft the required functional groups to the silicon surface. The disadvantage of the organosilicon reaction is the need to strictly control the anhydrous and oxygen-free conditions. In addition, in the subsequent step of modifying phenylboryl groups, the common method is to use compounds such as aminophenylboronic acid and tetravinylphenylboronic acid as raw materials to react with surface-modified functional groups. On the o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30B01D15/32
CPCB01D15/32B01J20/28009B01J20/286
Inventor 付华宋维君张爱华孙春艳刘霍宋浩宇陶政远王玉环马丽张研
Owner QINGHAI UNIVERSITY
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