Method for modifying nano metal oxide by coupling graft

A technology of nano-metal and graft modification, which is applied in the treatment of dyed organic silicon compounds, dyed low-molecular organic compounds, and fibrous fillers. Slow rate, low activity of organic long-chain molecules, etc., to achieve the effects of not easy side reactions, low cost, and high selectivity

Inactive Publication Date: 2010-11-10
CHONGQING UNIV
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  • Abstract
  • Description
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Problems solved by technology

However, the disadvantage of this method is that the activity of organic long-chain molecules, especially polymer terminal reactive groups, is low, and the reaction rate with high-activity groups on the surface of nanoparticles is slow, resulting in low grafting efficiency and poor modification. not effectively
For example, in the article "Preparation and carboxylation modification of monodisperse nano-silica microspheres" in the 11th issue (40) volume of "Functional Materials" in 2009, 3-aminopropyltriethoxysilane coupling agent and Succinic anhydride is used to modify the surface of nano-silica by carboxylation. Although a certain proportion of organic matter is grafted on the surface of nano-silica after modification, the grafting efficiency is still not high, and it cannot effectively solve the gap between nano-materials and organic matrix. Incompatibilities

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  • Method for modifying nano metal oxide by coupling graft
  • Method for modifying nano metal oxide by coupling graft
  • Method for modifying nano metal oxide by coupling graft

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as Figure 1~3 Shown, the concrete steps of a kind of method of coupling graft modification nano-metal oxide are as follows:

[0035] (1) Drying treatment of nanoparticles

[0036] Nano zinc oxide powder with an average particle size of 20nm was put into a high-temperature muffle furnace, and dried at 300° C. for 12 hours.

[0037] (2) Coupling reaction of nanoparticles

[0038] After the first step (1) is completed, first the nano-zinc oxide powder after the drying treatment of the (1) step and aminopropyltriethoxysilane coupling agent and toluene are added in the three-port reaction vessel, and the nano-zinc oxide The mass ratio of powder:aminopropyltriethoxysilane coupling agent:toluene is 1:0.02:50. Then feed high-purity nitrogen into the three-port reaction vessel to isolate the influence of oxygen in the air on the reaction, and heat the temperature of the mixed solution to 80 ° C. At the same time, open the circulating condensed water at the gas outlet of...

Embodiment 2

[0049] A kind of concrete steps of the method for coupling graft modification nano-metal oxide, with embodiment 1, wherein:

[0050] In step (1), the nanometer metal oxide powder used is nanometer titanium dioxide powder with an average particle diameter of 10 nm. The drying temperature was 400° C., and the drying time was 6 hours.

[0051] In the (2) step, the aminosilane coupling agent used is 2-aminoethylaminopropyl trimethoxysilane coupling agent, nanometer titanium dioxide powder: 2-aminoethylaminopropyl trimethoxysilane coupling agent The mass ratio of :toluene was 1:0.005:10, the temperature of the mixed solution was heated to 40° C., and the stirring time was 18 hours.

[0052] In step (3), the Soxhlet extraction time is 36 hours, the drying temperature is 100° C., and the drying time is 24 hours.

[0053] In the (4) step, the organic acid used is oleic acid, and the quality of oleic acid is 0.5 times of the quality of the 2-aminoethylaminopropyltrimethoxysilane coup...

Embodiment 3

[0058] A kind of concrete steps of the method for coupling graft modification nano-metal oxide, with embodiment 1, wherein:

[0059] In step (1), the nano metal oxide powder used is a nano silicon dioxide powder with an average particle diameter of 50 nm. The drying temperature was 100° C., and the drying time was 24 hours.

[0060] In the (2) step, the aminosilane coupling agent used is an aminoethylaminopropyltriethoxysilane coupling agent, wherein nano-silica powder: aminoethylaminopropyltriethoxysilane coupling The mass ratio of agent:toluene is 1:0.1:75, the temperature of the mixed solution is heated to 110° C., and the stirring time is 4 hours.

[0061] In step (3), the Soxhlet extraction time is 6 hours, the drying temperature is 270° C., and the drying time is 6 hours.

[0062] In the (4) step, the organic acid used is 12-hydroxy octadecanoic acid, and the quality of 12-hydroxy octadecanoic acid is that of the aminoethylaminopropyl triethoxysilane coupling agent add...

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Abstract

The invention discloses a method for modifying a nano metal oxide by coupling graft, and belongs to the technical field of nano granule surface modification. The nano metal oxide is used as a raw material, N,N'-carbonyl diimidazole (CDI) is used as an activating agent, and a finished product is obtained by simple processes of drying treatment, coupling reaction, separation and purification, coupling graft, re-separation and re-purification. The method has the advantages of simplicity, mild reaction conditions, high grafting efficiency which reaches 87 percent, energy conservation, emission reduction, low cost and suitability for large-scale industrial production. The nano metal oxide prepared by using the method can be widely applied in the fields of rubber, coating, ink, dye, glass, piezoelectric ceramics, photoelectrons, medicament and the like.

Description

technical field [0001] The invention belongs to the technical field of surface modification of nanoparticles, and in particular relates to a method for using N,N'-carbonyldiimidazole (CDI) to activate organic acid coupling and grafting to modify nanometer metal oxides. Background technique [0002] Due to the miniaturization of particle size, the specific surface area of ​​nanomaterials increases sharply, which makes nanomaterials produce surface effects, small size effects and macroscopic quantum tunneling effects that traditional materials do not have. Therefore, nanomaterials have many unique and excellent properties in magnetism, light, electricity, chemistry, physics and biology, etc., and have shown broad potential in the fields of rubber, coatings, inks, dyes, glass, piezoelectric ceramics, optoelectronics and medicine. Application prospect. [0003] Due to the small particle size and high proportion of surface atoms, nanomaterials have extremely high specific surfac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C3/08C09C3/12C09C1/04C09C1/28C09C1/36C09C1/40C09C1/00
Inventor 陈恒志贾玲玲
Owner CHONGQING UNIV
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