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Spherical silicon-based organic-inorganic hybrid boron adsorbent and preparation method thereof

A spherical silicon, adsorbent technology, applied in inorganic chemistry, chemical instruments and methods, adsorbed water/sewage treatment, etc., can solve the problems of uncontrollable group density, poor mechanical properties, mass transfer effects, etc., to facilitate industrial application , good mechanical properties, good stability

Active Publication Date: 2014-06-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

1) Since most of these adsorbents are organic polymers, they are easy to swell and shrink after repeated adsorption-regeneration cycles in a strong acid and strong alkali environment, resulting in broken adsorbents, poor mechanical properties, and difficult to regenerate and reuse
2) Organic polymer resin, whose skeleton is mostly composed of polystyrene or divinylbenzene copolymer, has strong hydrophobicity, especially the structure contains benzene ring, and its non-polar structure enhances hydrophobicity, which is not conducive to the water environment The mass transfer and diffusion of medium solute, so the mass transfer is not effective in boric acid aqueous solution, which affects the adsorption kinetics and equilibrium adsorption capacity
3) This kind of adsorbent is produced by the modification of functional groups grafted on the polymer skeleton, and the group density cannot be controlled, so the group density will be lower, resulting in lower adsorption capacity
However, the shape of this silicon-based boron adsorbent is amorphous particles formed by drying the bulk gel and grinding it, which will affect the fluid distribution and adsorption kinetics
During the adsorption process, the amorphous form will significantly change the linear velocity of the fluid and the state of the push flow, make the fluid distribution unbalanced, form a channeling effect, and affect the mass transfer, resulting in a sudden change or decrease in the dynamic adsorption amount, and the adsorption Balance rate reduction
At the same time, the amorphous form is easy to wear, so that the pressure drop of the bed layer increases, which is not convenient for solid-liquid separation, and is not conducive to industrial application

Method used

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  • Spherical silicon-based organic-inorganic hybrid boron adsorbent and preparation method thereof
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  • Spherical silicon-based organic-inorganic hybrid boron adsorbent and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0054] (1) Preparation of precursor: Mix meglumine as a polyhydroxy functional compound with γ-(2,3-epoxypropoxy)propyltrimethoxysilane at a molar ratio of 1:1, add N,N-dimethyl Dissolve the base formamide solvent until it is completely dissolved, stir the reaction at 80°C for 4 hours, import the reacted solution into a rotary evaporator, and remove the solvent at 60°C at 200r / min for 20min, and extract the residue by Soxhlet (Using methanol as the reflux extraction solution, extracting at 70°C) After 48 hours, a precursor containing boron-selective functional groups was obtained;

[0055] (2) Preparation of sol: Take 0.5 g of the precursor prepared in step (1) and 2.0 g of tetramethoxysilane, dissolve them in 10 ml of 50% methanol aqueous solution, add hydrochloric acid to adjust the pH to 2, and store the resulting mixture at 80°C The reaction was carried out for 12 hours, and the sol was obtained after the end of the reaction;

[0056] (3) Preparation of spherical silicon-...

Embodiment 2

[0060] (1) Preparation of precursor: Meglumine is used as a polyhydroxy functional compound, mixed with γ-(2,3-glycidoxy)propyltrimethoxysilane at a molar ratio of 1:1, and N,N-di Methylformamide is dissolved in a solvent until it is completely dissolved, and the reaction is stirred at 80°C for 4 hours, and the reacted solution is introduced into a rotary evaporator, and at 60°C, 200r / min rotary evaporator for 20min to remove the solvent, and the residue is subjected to Soxhlet After 48 hours of extraction (using methanol as the reflux extraction solution at 70°C), a precursor containing boron-selective functional groups was obtained;

[0061] (2) Preparation of sol: Take 1.0 g of the precursor prepared in step (1) and 1.0 g of tetramethoxysilane, dissolve them in 10 ml of 50% methanol aqueous solution, add hydrochloric acid to adjust the pH to 2, and store the resulting mixture at 80°C Reacted for 12 hours, and the sol was obtained after the reaction;

[0062] (3) Preparatio...

Embodiment 3

[0065] (1) Preparation of precursor: Meglumine was used as a polyhydroxy functional group compound, and γ-(2,3-glycidoxy)propyltrimethoxysilane was dissolved in N,N-dimethoxysilane at a molar ratio of 1:1. In methylformamide solvent, stirred and reacted at 80°C for 4 hours, introduced the reacted solution into a rotary evaporator, and at 60°C, 200r / min rotary evaporator for 20min to remove the solvent, and the residue was extracted by Soxhlet (with methanol After 48 hours, the precursor containing boron-selective functional groups was obtained;

[0066] (2) Preparation of sol: Take 2.5 grams of the precursor prepared in step (1) and 0.5 grams of tetramethoxysilane, dissolve them in 10 ml of 50% methanol aqueous solution, add hydrochloric acid to adjust the pH to 2, and store the resulting mixture at 80°C Reacted for 12 hours, after the reaction ended, a sol was obtained;

[0067] (3) Preparation of spherical silicon-based boron adsorbent: Add the sol prepared in step (2) into...

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Abstract

The invention discloses a spherical silicon-based organic-inorganic hybrid boron adsorbent. The main component of the adsorbent is an inorganic substance; the adsorbent is good in mechanical property and the finished product of the adsorbent is a sphere good in uniformity. The invention further discloses a preparation method of the adsorbent. The preparation method comprises the following steps: (1) dissolving meglumine and organosilane with an epoxy group into polar solvent, reacting, distilling and purifying to obtain a precursor; (2) dissolving the precursor obtained in the step (1) and organosilane with a methoxy group or an ethoxy group in a water solution of alcohol in the molar ratio of (0.25-10):1, adding dilute acid to adjust the pH value to 1-4, and carrying out hydrolysis and condensation polymerization to obtain sol; and (3) adding the sol obtained in the step (2) and a surfactant with the volume accounting for 0.02-1% of the volume of the sol into dispersing solvent with the volume 1-20 times the volume of the sol while stirring to obtain a reaction system, carrying out cross-linking reaction at aging temperature, carrying out solid-liquid separation after the cross-linking reaction, washing and drying the separated solid to obtain the spherical silicon-based organic-inorganic hybrid boron adsorbent.

Description

technical field [0001] The invention relates to a preparation technology of a boron adsorbent, in particular to a spherical silicon-based organic-inorganic hybrid boron and a preparation method thereof. Background technique [0002] Boron is an extremely important metal resource and has very high economic value in many fields such as national defense, building materials, machinery, chemical industry, medicine, and agriculture. However, boron resources are increasingly scarce, and solid boron ore has been increasingly exhausted after mining. Therefore, the separation and extraction of boron from liquid boron ore, especially salt lake brine, has great research value. In addition, boron is an essential element in life such as plants and animals, but when the content exceeds the required range, it will produce toxic side effects. The international drinking water standard stipulates that the boron content in drinking water should not exceed 1.0 mg / L. According to the "Hygienic ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F1/58
Inventor 鲍宗必张茜任其龙邢华斌苏宝根杨亦文张治国
Owner ZHEJIANG UNIV