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Method for preparing micro-nano hybrid mesoporous adsorbing microspheres by utilizing red attapulgite clay

A technology of attapulgite clay and adsorption microspheres, applied in chemical instruments and methods, inorganic chemistry, alkali metal compounds, etc., to achieve the effects of high-value utilization, easy process control, and simple process

Active Publication Date: 2016-06-15
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

We have also used the hydrothermal method to make the short-diameter attapulgite long-diameter (patent CN103086392A), but in the red attapulgite clay, attapulgite rod crystals and associated mineral crystals are transformed, thereby obtaining amorphous mesoporous adsorption In terms of microspheres, there are currently no relevant research reports at home and abroad.

Method used

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  • Method for preparing micro-nano hybrid mesoporous adsorbing microspheres by utilizing red attapulgite clay
  • Method for preparing micro-nano hybrid mesoporous adsorbing microspheres by utilizing red attapulgite clay
  • Method for preparing micro-nano hybrid mesoporous adsorbing microspheres by utilizing red attapulgite clay

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Mix 100g of attapulgite clay mineral powder with 10g of sodium silicate and grind for 4 hours, then heat-treat with microwave at 140°C for 0.5; disperse the obtained product into 800mL of an aqueous solution containing 0.25g of citric acid, and then add 7.5 150mL aqueous solution of 1g magnesium chloride and 2.5g zinc chloride, fully stirred, transferred to a 2L hydrothermal reaction kettle, reacted at 260°C for 48h, and cooled to room temperature at 10°C / min; the solid product was separated, washed with water, and vacuum After drying and crushing, the off-white adsorption material was obtained.

Embodiment 2

[0024] Example 2: Mix 100g of attapulgite clay mineral powder with 100g of potassium metasilicate, grind for 4h, then heat-treat with microwave at 80°C for 4h; disperse the obtained product into 800mL of an aqueous solution containing 2g of ethylenediaminetetraacetic acid, and then Add 150mL of aqueous solution containing 60g of magnesium nitrate and 20g of zinc nitrate, stir well, transfer to a 2L hydrothermal reaction kettle, react at 160°C for 2h, and cool down to room temperature at 10°C / min; separate the solid product, wash with water, Vacuum dried and crushed to obtain off-white adsorption material.

Embodiment 3

[0025] Example 3: Mix 100g of attapulgite clay mineral powder with 50g of sodium potassium silicate and grind for 4 hours, then heat it with microwave at 100°C for 1 hour; disperse the obtained product into 800mL of aqueous solution containing 0.5g of oxalic acid, and then add 49.5 150 mL of aqueous solution of 1 g of magnesium acetate and 0.5 g of zinc acetate, stirred well, transferred to a 2L hydrothermal reaction kettle, reacted at 180°C for 24 hours, and cooled to room temperature at 10°C / min; the solid product was separated, washed with water, and vacuum After drying and crushing, the off-white adsorption material was obtained.

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Abstract

The invention discloses a method for preparing micro-nano hybrid mesoporous adsorbing microspheres by utilizing red attapulgite clay. The method comprises the steps of mixing the read attapulgite clay with silicate, and grinding, performing microwave heating at 80 to 140 DEG C, and activating for 0.5 to 4h; dispersing the obtained solid into an organic acid aqueous solution according to the solid-to-liquid ratio of 1 to 9.5, then adding a metal salt water solution, and uniformly stirring; transferring the obtained suspension liquid into a hydrothermal reactor provided with a tetrafluoroethylene liner, reacting at temperature of 160 to 260 DEG C for 2 to 48h, and cooling to the normal temperature at the speed of 10 DEG C / min; performing separating, washing, drying and smashing on a product to obtain the adsorbing microspheres. According to the method disclosed by the invention, the red attapulgite clay with abundant reserves, low grade and deep color and luster is subjected to treatment to obtain a spherical amorphous silicate adsorbing material with the mesoporous structure, and a product is large in specific surface area, uniform in pore diameter distribution, can be used for adsorption and enrichment or desorption of antibiotic, mycotoxin, dye and heavy metal, and has a wide application prospect in environmental restoration, wastewater treatment and feed additives.

Description

technical field [0001] The invention relates to a method for preparing micro-nano hybrid mesoporous adsorption microspheres by using red attapulgite clay, and belongs to the technical field of deep processing of natural non-metallic minerals and preparation of nanometer materials. Background technique [0002] Attapulgite clay (also known as palygorskite or palygorskite) is a hydrous magnesium-aluminosilicate clay mineral with attapulgite as the main component. It has nanorod crystal morphology and abundant nanopores. Therefore, it has a large specific surface area and exhibits excellent adsorption performance. Attapulgite clay resources are abundant in my country. Attapulgite clay deposits were first discovered in the Jiangsu and Anhui regions. In recent years, iron-rich attapulgite clay deposits have also been discovered in Zhangye, Huining, Huangshui, and Hangjin Banner, Inner Mongolia. Due to the rich iron in the crystal skeleton, it is red or brick red, but it has not ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/12B01J20/28B01J20/30
CPCB01J20/10B01J20/12B01J20/28021B01J20/28064B01J20/28083
Inventor 王文波王爱勤田光燕宗莉康玉茹
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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