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Attapulgite particle with aromatic tertiary amine structure on surface and preparation method of attapulgite particle

A technology of attapulgite and aromatic tertiary amine, which is applied in the field of functionalized attapulgite particles and its preparation, can solve the problems of attapulgite with large specific surface area, poor affinity of polymers, and easy agglomeration, so as to improve value and Utilization rate, reduction of dispersion size, and improvement of dispersion

Inactive Publication Date: 2015-04-22
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large specific surface area of ​​attapulgite, it is easy to agglomerate, and the surface contains polar hydroxyl groups, which has poor affinity with polymers, so it can only be used as a filler.
In order to exert its excellent performance, the traditional method is to treat the attapulgite with a coupling agent. After the treatment with the coupling agent, the dispersion of attapulgite in the polymer is improved, but it still cannot achieve nanoscale dispersion, and the agglomeration phenomenon remains serious

Method used

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  • Attapulgite particle with aromatic tertiary amine structure on surface and preparation method of attapulgite particle
  • Attapulgite particle with aromatic tertiary amine structure on surface and preparation method of attapulgite particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 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.

[0028] Disperse the purified attapulgite in 1 mol / L hydrochloric acid and vibrate ultrasonically for 6 minutes, remove the solvent after standing for 24 hours, wash until neutral, dry in vacuum, grind and sieve to obtain acid-activated attapulgite.

[0029] 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 surfa...

Embodiment 2

[0032] 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.

[0033] 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.

[0034] 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.

[0035] Disperse 1...

Embodiment 3

[0037] 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.

[0038] 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.

[0039] Take 4g of acid-activated attapulgite soil and disperse it in 100mL of ethylene glycol, disperse it ultrasonically for 40min, add 8γ-aminopropylmethyldiethoxysilane dropwise under the condition of stirring, after the dropwise addition, heat to 180°C, and react After 6 hours of reaction, the solvent was removed, vacuum-dried, ground and sieved to obtain attapulgite with amino groups bonded to the surface.

[0040]...

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Abstract

The invention relates to an organic attapulgite particle with an aromatic tertiary amine structure on the surface, and a preparation method of the organic attapulgite particle. The preparation method comprises the following steps: firstly, introducing primary amine into the surface of the attapulgite through dealcoholization reaction of the alcoxyl of the alkoxy silane of the primary amine with hydroxyl on the surface of the attapulgite; secondly, forming a stable Schiff base through dehydration of the primary amine with 4-(diethylin) salicylaldehyde so as to prepare the functional attapulgite particle of which the surface is bonded with the aromatic tertiary amine structure, wherein the bonding quantity of the aromatic tertiary amine on the surface of the attapulgite is as high as 1.53 mmol / g. The application range of the attapulgite is widened; the prepared functional attapulgite particle of which the surface is bonded with the aromatic tertiary amine structure can be used for establishing an oxidation-reduction initiating system with organic peroxy-initiators such as peroxy-diphenyl diketone; and attapulgite / allyl monomer polymer hybridization particles is prepared through surface initiation graft polymerization reaction in an organic solvent, so that preconditions are created for the additional values of the attapulgite.

Description

technical field [0001] The invention relates to a functionalized attapulgite particle with an aromatic tertiary amine structure on the surface and a preparation method thereof. Background technique [0002] Attapulgite clay is a kind of water-containing natural nano-layered clay mineral with attapulgite as the main component, rich in three metal elements of magnesium, aluminum and silicon. The basic structure of attapulgite makes it a natural one-dimensional rod-shaped nanomaterial, which exhibits various excellent physical and chemical properties, such as adsorption and reinforcement, and can be widely used in industrial fields. Because attapulgite has a large specific surface area, it is easy to agglomerate, and the surface contains polar hydroxyl groups, which has poor affinity with polymers, so it can only be used as a filler. In order to exert its excellent performance, the traditional method is to treat the attapulgite with a coupling agent. After the treatment with t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/40
Inventor 龚方红刘惠杨海存倪庆婷陶国良
Owner CHANGZHOU UNIV
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