Industrial preparation method of anionic resin loaded nano zirconia composite material

A technology of nano-zirconia and anion resin, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problem of reducing the utilization efficiency of nano-particle sites, high energy consumption of evaporation and concentration, and carrier pores Problems such as clogging can be avoided, and the effects of reducing cost and energy consumption, less environmental pollution, and less pore clogging can be achieved.

Active Publication Date: 2020-01-17
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method can be applied to the gram-level preparation of anionic resin-based nano-zirconia, but it is difficult to apply to industrial production due to the high energy consumption of evaporation and concentration and high equipment requirements.
Chinese invention patent (application publication number CN107262072A, publication date: October 20, 2017) discloses an industrial preparation method of zirconium-loaded nanocomposite resin adsorbent, which solves the problem of laboratory preparation methods being directly extended to The heat transfer, mass transfer, flow and other problems faced in industrial scale production have initially met the needs of industrial preparation, but heating is still required in the salt immersion stage of the resin, which consumes a lot of energy and requires high equipment requirements; more important Unfortunately, due to the strong electrostatic repulsion between the zirconium salt ions and the resin matrix during the loading process, the loading effect of this method is still not good, and excessive zirconium salt needs to be added to force the hydrated zirconium cations into the resin, resulting in nano-zirconia Concentrated on the periphery of the resin carrier, the nanoparticles are obviously agglomerated, and the pores of the carrier are severely blocked, which reduces the site utilization efficiency of the nanoparticles

Method used

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  • Industrial preparation method of anionic resin loaded nano zirconia composite material
  • Industrial preparation method of anionic resin loaded nano zirconia composite material
  • Industrial preparation method of anionic resin loaded nano zirconia composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The preparation method of the present embodiment comprises the following steps:

[0030] (1) Resin transformation: wash and dry 20kg of commercially available D201 resin, add it to 40L of 10% (w / w) NaOH solution, stir at 300rpm for 2 hours, then leach out and recover the lye;

[0031] (2) Preparation of zirconium alcohol feed solution: 24kg zirconium oxychloride octahydrate (commercially available) was dissolved in 40L methanol, stirred at a speed of 300rpm for 1h, and the alcohol solution of zirconium was prepared as feed solution for later use, wherein the concentration of zirconium was about 170g / L (zirconium / alcohol);

[0032] (3) Primary precipitation: Add the transformed resin in step (1) into the zirconium alcohol material liquid prepared in step (2), stir at a speed of 300 rpm, and react for 3 hours to complete the primary precipitation of zirconia in the resin, and the zirconium liquid Recycle;

[0033] (4) Secondary precipitation: Leach out the material afte...

Embodiment 2

[0038] The preparation method of this example is similar to Example 1, but the D201 resin in step (1) is replaced by D301 resin, whose skeleton is polystyrene-divinylbenzene, tertiary amino group.

[0039] The nanocomposite material that present embodiment makes is spherical, and diameter is 0.6-0.8mm, and moisture content is 48% (v / v), records zirconium loading amount by inductively coupled plasma optical emission spectrometer (ICP-OES) after drying was 12.1%.

[0040] This example proves that in this invention, different anion exchange resins can be used as carriers, all of which can achieve better loading effects.

Embodiment 3

[0042] The preparation method of this example is similar to Example 1, but the 40L 10% (w / w) NaOH solution in step (1) is replaced by 40L 5% (w / w) NaOH solution.

[0043] The nanocomposite material that present embodiment makes is spherical, and diameter is 0.6-0.8mm, and moisture content is 45% (v / v), records zirconium loading amount by inductively coupled plasma optical emission spectrometer (ICP-OES) after drying was 10.8%.

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Abstract

The invention discloses an industrialized preparation method of an anionic resin-loaded nano zirconia composite material. The main preparation steps include: (1) adding anion exchange resin into alkali liquor, stirring and reacting to convert the resin into OH type, and washing with water to neutrality for later use; (2) dissolving zirconium salt in alcohol to prepare feed liquid for later use; (3) adding the material into the feed liquid, stirring and taking out after fully reacting; (4) adding alkali liquor, stirring, taking out after reaction, soaking with acid liquor, flushing with tap water to neutrality, and bagging; and (5) after the chemicals are added to the feed liquid and lye, directly applying to the next batch of production. The method has the advantages of simple process, noneed of heating and drying, short time consumption and low cost, and can effectively overcome the problem the nano zirconia is not easily loaded in anionic resin; the obtained product has stable zirconium loading amount and excellent decontamination performance, the large-scale production efficiency of the anion resin loaded nano zirconium oxide composite material is greatly improved, and the method has strong economic benefits and environmental protection benefits.

Description

technical field [0001] The invention belongs to an industrial preparation method of an anionic resin-loaded nano-zirconia composite material. Background technique [0002] There are a large number of inorganic anion pollutants in drinking water and sewage, such as phosphorus (phosphate, phosphite, hypophosphite, hyperphosphate, etc.), arsenic (arsenate, arsenite, etc.), fluoride, bromide , Selenate, etc. Some of these pollutants are highly toxic (such as arsenic, fluorine, bromine, selenium, etc.), which can easily cause damage to humans and other organisms; the other part is easy to cause eutrophication of water bodies (such as phosphorus, etc.), affecting water bodies. use value. For the above pollutants, scholars at home and abroad have developed and applied a variety of methods, including precipitation, electrocoagulation, membrane separation and adsorption. Among them, the adsorption method has been widely concerned and applied due to its advantages such as high remo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/30B01J20/32C02F1/28
CPCB01J20/06B01J20/3085B01J20/321B01J20/3236C02F1/288
Inventor 张孝林方卓尧潘丙才邓子牛
Owner NANJING UNIV
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