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Nano-hydroxyapatite/polyhexamethylene monoguanidine hydrochloride/silica gel composite material preparation method and solid-phase extraction method

A technology of polyhexamethylene monoguanidine hydrochloride and nano-hydroxyapatite, which is applied to the preparation of nano-hydroxyapatite/polyhexamethylene monoguanidine hydrochloride/silica gel composite materials, solid phase extraction of traces in water In the field of quantitative Cr, it can solve the problems of low mechanical strength, small particle size of nanomaterials, and large flow resistance, and achieve the effects of non-toxic and harmless raw materials, high adsorption efficiency, and simple preparation methods

Active Publication Date: 2020-10-16
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small particle size of nanomaterials, the flow resistance in solid phase extraction is large, and there are often problems such as easy loss and easy blockage of pipelines.
To solve this problem, nanomaterials are often loaded on the carrier, such as carbon nanotubes loaded on silica gel, which solves the problem of flow resistance, but only by physical adsorption loading method, the mechanical strength is not high

Method used

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  • Nano-hydroxyapatite/polyhexamethylene monoguanidine hydrochloride/silica gel composite material preparation method and solid-phase extraction method
  • Nano-hydroxyapatite/polyhexamethylene monoguanidine hydrochloride/silica gel composite material preparation method and solid-phase extraction method

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Experimental program
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Effect test

Embodiment 1

[0025] The preparation method of nano-hydroxyapatite / polyhexamethylene monoguanidine hydrochloride / silica gel composite material comprises the following specific steps:

[0026] (1) Weigh 6.0g of silica gel with a particle size of 80-100 mesh and put it into a 100mL beaker, add 60mL of 2.5mol / L nitric acid solution, stir for 30 minutes, seal, soak for 16 hours, filter, and wash with deionized water until neutral , Dry at 150°C for 4 hours.

[0027] (2) Weigh 80.0 mg of activated silica gel into a 10 mL centrifuge tube, add 10 mL of polyhexamethylene monoguanidine hydrochloride solution with an average molecular weight of about 2000 and a concentration of 1.0%, shake well, and ultrasonically shake for 10 minutes, then add 16.0 mg of nano-hydroxyapatite with a particle size of 20-50nm, that is, the mass ratio of nano-hydroxyapatite to silica gel is 1:5, shake well, and then ultrasonically vibrate for 10 minutes, centrifuge for 20 minutes (centrifuge rotation speed 10000 rpm / mi...

Embodiment 2

[0029] Take 20 mg of the composite material prepared in Example 1 and put it into a self-made micro-enrichment column. The micro-enrichment column has an inner diameter of 2.0 mm and a polytetrafluoroethylene tube with a length of 4.0 cm. Connect a peristaltic pump to adjust the pH of the water sample to 4.0. At a sampling flow rate of 3.5mL / min, 40mL of water samples were enriched, and then eluted with 1mL 8% (v / v) nitric acid solution at an elution flow rate of 6.5mL / min, and the eluate was analyzed by atomic absorption spectrometry Measure with a photometer and record the absorbance value. The standard curve method was used to determine the content of Cr(Ⅵ) in water.

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Abstract

The invention relates to a method for preparing a nano-hydroxyapatite / polyhexamethylene monoguanidine hydrochloride / silica gel composite material. The salt load is prepared on silica gel. First, the silica gel is activated, and then the mass ratio of nano-hydroxyapatite to activated silica gel is 1:5-1:30, and polymethylene monosodium chloride with a concentration of 0.25-1.0% is added. Guanidine hydrochloride solution, ultrasonic vibration, centrifugation, and drying in a vacuum oven to obtain the finished product. The invention is a solid-phase extraction adsorption material, which avoids the disadvantages of easy loss and blockage of pipelines during use of a single nanometer material. The enrichment effect on Cr(Ⅵ) is ideal, and it can be used for speciation analysis of chromium in environmental water samples. Reusable at least 20 times.

Description

technical field [0001] The invention relates to a solid-phase extraction material, in particular to a method for preparing a nano-hydroxyapatite / polyhexamethylene monoguanidine hydrochloride / silica gel composite material and a method for solid-phase extraction of trace Cr(VI) in water. Background technique [0002] The accurate determination of trace heavy metal element chromium and its form in water is an important indicator of water quality detection. Due to the low content of chromium in water and the matrix interference of coexisting salts, etc. have always been problems that need to be solved in water quality testing. In this case, the separation and enrichment of samples is an essential step. Solid phase extraction is one of the commonly used sample pretreatment techniques. Because of the variety of adsorption materials that can be selected, it has attracted extensive research by scholars. At present, it is a hotspot in the research of solid-phase extraction technol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/30B01D15/10G01N1/40G01N21/31
CPCB01D15/10B01J20/281G01N1/40G01N21/3103
Inventor 李成威于洪梅占美红刘岐
Owner UNIV OF SCI & TECH LIAONING
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