Functional attapulgite particle with amido on surface and preparation method thereof

A technology of attapulgite and amino, which is applied in the field of attapulgite particles and its preparation, which can solve the problems of ineffective combination of attapulgite and polymer properties, serious agglomeration, and difficulty in effective dispersion, so as to increase added value and resources The effect of utilization

Inactive Publication Date: 2013-03-27
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The surface and interior of attapulgite contain a large amount of silicon hydroxyl, magnesium hydroxyl, aluminum hydroxyl, and three kinds of water, zeolite water, structural water and crystal water, which make attapulgite very hydrophilic, so that it is easy to dissolve in polymer systems. Aggregation, difficult to effectively disperse, can n

Method used

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  • Functional attapulgite particle with amido on surface and preparation method thereof
  • Functional attapulgite particle with amido on surface and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Disperse 10g of attapulgite containing impurities in 100mL of distilled water, disperse by ultrasonic for 60min, add 0.2g of sodium hexametaphosphate, heat to 70°C, stir for 4h, pour out the upper suspension, remove the solvent, wash several times, vacuum dry, and grind Sieve to obtain purified attapulgite.

[0025] Disperse the purified attapulgite in 1 mol / L hydrochloric acid and vibrate ultrasonically for 6 hours, remove the solvent after standing for 24 hours, wash until neutral, dry in vacuum, grind and sieve to obtain acid-activated attapulgite.

[0026] Take 4g of acid-activated attapulgite soil and disperse it in 100mL of toluene, ultrasonically disperse for 60min, add 8g of γ-aminopropyltriethoxysilane dropwise under stirring condition, after the dropwise addition, heat to 80°C, react for 12h, and the reaction ends Afterwards, the solvent is removed, vacuum-dried, ground and sieved to obtain attapulgite with primary amino groups chemically bonded to the surface...

Embodiment 2

[0028] Disperse 10g of attapulgite containing impurities in 200mL of distilled water, ultrasonically disperse for 30min, add 0.2g of sodium hexametaphosphate, heat to 80°C, stir for 6h, pour out the upper suspension, remove the solvent, wash several times, vacuum dry, and grind Sieve to obtain purified attapulgite.

[0029] Disperse the purified attapulgite in 0.5 mol / L dilute sulfuric acid and vibrate it ultrasonically for 30 minutes, remove the solvent after standing for 24 hours, wash until neutral, dry in vacuum, grind and sieve to obtain acid-activated attapulgite.

[0030] Take 4g of acid-activated attapulgite soil and disperse it in 150mL of toluene, ultrasonically disperse for 30min, add 4g of γ-aminopropyltrimethoxysilane dropwise under stirring condition, after the dropwise addition, heat to 110°C, react for 10h, after the reaction , remove the solvent, vacuum dry, grind and sieve to obtain the attapulgite with amino groups bonded to the surface.

Embodiment 3

[0032] Disperse 10g of impurity-containing attapulgite in 250mL of distilled water, disperse by ultrasonic for 40min, add 0.1g of sodium hexametaphosphate, heat to 60°C, stir for 5h, pour out the upper suspension, remove the solvent, wash several times, vacuum-dry, and grind Sieve to obtain purified attapulgite.

[0033] Disperse the purified attapulgite in 1 mol / L hydrochloric acid and vibrate ultrasonically for 40 minutes, let it stand for 24 hours, remove the solvent, wash until neutral, dry in vacuum, grind and sieve to obtain acid-activated attapulgite.

[0034] Take 4g of acid-activated attapulgite soil and disperse it in 100mL of ethylene glycol, disperse it ultrasonically for 40min, add 8N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane dropwise under stirring condition, drop After the addition, heat to 180°C and react for 6 hours. After the reaction, remove the solvent, dry in vacuum, grind and sieve to obtain the attapulgite with amino groups bonded to the surface....

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Abstract

The invention relates to a functional attapulgite particle with amido on a surface and oxidation-reduction initiation activity and a preparation method thereof. The preparation method comprises the following steps: purifying attapulgite raw ores; then carrying out acid activation; finally dispersing attapulgite subjected to the acid activation and amido alkoxy silane into an organic solvent, carrying out back flowing under the condition of 110-180 DEG C for 6-12 hours, and filtering, washing, drying and smashing products after reaction is finished to obtain the product. The preparation method disclosed by the invention grafts the amido alkoxy silane to the surface of the attapulgite through chemical bonding by adopting a dealcoholization method, thereby overcoming the defects of reduced coupling efficiency, which is caused due to the polycondensation reaction of silicon hydroxyl in a hydrolization method, of the traditional coupling agent; and the prepared functional attapulgite particle disclosed by the invention achieves high amido content of 5.82 mmol/g on the surface, can be used for initiating the polymerization reaction through surface initiation graft polymerization reaction and creates the precondition for the additional value of the attapulgite.

Description

technical field [0001] The invention relates to attapulgite particles with amino groups on the surface and oxidation-reduction initiation activity and a preparation method thereof. Background technique [0002] Attapulgite clay is a kind of water-containing natural nano-layered clay mineral with Attapulgite (AT for short) as the main component, rich in three metal elements of magnesium, aluminum and silicon. Its crystal structure is fibrous or narrow-banded with a high aspect ratio, which varies according to the place of origin. In addition to attapulgite, it often contains montmorillonite, kaolinite, hydromica, sepiolite, quartz, Minerals such as opal and carbonate. Attapulgite is a natural mineral nanomaterial with good adsorption, decolorization, ion exchange, thermal stability, salt resistance, gelling, pulping and high-temperature phase transition properties, and can be widely used in petroleum, chemical, geological and pharmaceutical fields . Attapulgite is a natura...

Claims

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Application Information

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IPC IPC(8): C01B33/40
Inventor 龚方红杨海存刘惠倪庆婷刘春林
Owner CHANGZHOU UNIV
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