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Nano diamond derivative with end group as amino group as well as preparation method and application thereof

A nano-diamond and end-group technology is applied in the field of nano-diamond derivatives and the preparation of derivatives to achieve the effects of high technology content, stable chemical structure and good solubility

Inactive Publication Date: 2013-06-26
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the above-mentioned nano-diamond derivatives whose terminal groups are amino groups and their preparation methods have not yet been published in the public literature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A nano-diamond derivative whose amino group has an amino group content of about 0.1% is an amino group, and the specific preparation method is as follows:

[0041] 1) Purify and oxidize the nano-diamond first: take 100g of nano-diamond, soak it in 40wt% hydrofluoric acid aqueous solution and reflux for 48 hours, filter it, wash it with running water, and dry it; in 2M HNO 3 Sonicate in the solution for 36 hours, reflux for 48 hours, filter, and wash with running water; then sonicate for 10 hours in an aqueous solution of OP-10 with a pH of 10 and a concentration of 30wt%, filter, and wash with running water. After repeating twice, immerse in 3M In HCl solution, sonicate for 24 hours, filter, wash with running water, and dry; after sonicating for 72 hours in concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 1:1, reflux for 96 hours, centrifuge, wash with running water, and dry for later use;

[0042] 2) Take 50g of nano-diamond after purifica...

Embodiment 2

[0052] A kind of nano-diamond derivative whose amino group has an amino group content of about 0.01% is an amino group, and its specific preparation method is as follows:

[0053] 1) Purify and oxidize the nano-diamond first, and the pretreatment method is the same as that of the above-mentioned embodiment 1;

[0054] 2) Take 50g of nano-diamond that has been purified and oxidized with mixed acid, add it to 600ml of thionyl chloride, sonicate in a 200kHz, 500W ultrasonic instrument for 24h, reflux at 80°C for 48h, and then centrifuge at 6000rpm for 10min to separate chlorine sulfoxide, washed with tetrahydrofuran, and vacuum-dried at room temperature for 24 hours;

[0055] 3) Take 25g of nano-diamonds containing acid chloride groups on the surface prepared in step 2) and 300g of 1,6-hexanediamine, and add them to 1000ml of N,N'-dimethylformamide respectively, under nitrogen protection, in After ultrasonication for 24 hours in a 200kHz, 500W ultrasonic instrument, stir at 95°C...

Embodiment 3

[0064] The content of a kind of amino group is about 0.04% and the end group is the nano-diamond derivative of amino group, and its specific preparation method is as follows:

[0065] 1) Purify and oxidize the nano-diamond first, and the pretreatment method is the same as that of the above-mentioned embodiment 1;

[0066] 2) Take 50g of nano-diamond after purification and mixed acid oxidation treatment, add it to 600ml of thionyl chloride, sonicate in a 200kHz, 500W ultrasonic instrument for 24h, reflux at 80°C for 48h, and then centrifuge at 6000rpm for 10min to separate chlorine sulfoxide, washed with tetrahydrofuran, and vacuum-dried at room temperature for 24 hours;

[0067] 3) Take 25g of nano-diamonds containing acid chloride groups on the surface prepared in step 2) and 300g of 1,3-propanediamine, and add them to 1000ml of N,N'-dimethylformamide respectively, under nitrogen protection, in After ultrasonication at 200kHz, 500W for 24 hours, stir at 95°C for 72 hours, th...

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Abstract

The invention relates to a nano diamond derivative with an end group as an amino group as well as a preparation method and an application thereof, and belongs to the field of nanometer materials. The derivative is prepared according to the following steps: firstly, reacting nano diamond subjected to purification and mixed acid oxidization treatments with thionyl chloride; then respectively carrying out nucleophilic substitution reaction on the product obtained from the former step and a diamine compound and trichloro-triazine; and then, utilizing the substituted nano-diamond to carrying out iteration reaction on the product obtained from the former step and the diamine compound and the trichloro-triazine, thus obtaining the derivative, wherein the amino content is about 0.01%-0.1%. The nano diamond derivative with the end group as the amino group has good dissolubility in an organic solvent, so that the nano diamond is stably dispersed; the preparation conditions of the derivative are easy to satisfy, and raw materials are available; the method for preparing the nano diamond derivative with the end group as the amino group through step-by-step iteration reaction is developed; and the derivative has high scientific and technological content, strong innovativeness and a good application prospect.

Description

technical field [0001] The invention relates to a nano-diamond derivative, in particular to a nano-diamond derivative whose terminal group is an amino group, as well as a preparation method and application of the derivative, belonging to the field of nanometer materials. Background technique [0002] Due to the quantum size effect and surface effect of nanomaterials, as well as the high hardness and wear resistance of diamond itself, nanodiamond has great application value in the fields of lubrication and ultra-precision polishing. Tests have shown that adding an appropriate amount of ultra-dispersed diamond particles to lubricating oil can reduce the friction coefficient by 10-50%, and reduce the wear by 1 / 3-1 / 4 (Zhang Shuda, Ji Degang, Song Lanting, Construction Machinery, 6, 31, 2005 ). However, due to the large specific surface and high specific surface energy of nano-diamonds, they are in a thermodynamically unstable state, and are easy to agglomerate to form massive a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M159/12C10M177/00C10N30/06
Inventor 柯刚谭湘倩浣石黄风雷
Owner GUANGZHOU UNIVERSITY
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