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Nanodiamond derivative having hydroxy groups as terminal groups, and preparation method and use thereof

A technology of nano-diamond and terminal group, which is applied in the field of preparation of nano-diamond derivatives and derivatives, achieving the effects of high technological content, easy acquisition and stable chemical structure

Inactive Publication Date: 2013-06-12
浣石
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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 end groups are hydroxyl groups and their preparation methods have not yet been published in the literature.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of nano-diamond derivative whose hydroxyl content is about 0.001% and whose terminal group is hydroxyl, the specific preparation method is as follows:

[0041] 1) Purify and oxidize the nano-diamond first: take 150g of nano-diamond, soak it in 40wt% hydrofluoric acid aqueous solution and reflux for 50h, filter it, wash it with running water, and dry it; in 2M HNO 3 Sonicate in the solution for 40 hours, reflux for 60 hours, filter, and wash with running water; then sonicate for 15 hours in an aqueous solution of OP-10 with a pH of 10 and a concentration of 30wt%, filter, and wash with running water for 3 times, then immerse in 3M In HCl solution, sonicate for 30 hours, filter, wash with running water, and dry; after sonicating for 48 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;

[0042] 2) Take 100g of purified and mixed-acid oxidation-treated nano-d...

Embodiment 2

[0051] The content of a kind of hydroxyl group is about 0.0035% and the end group is the nano-diamond derivative of hydroxyl group, and its specific preparation method is as follows:

[0052] 1) Purify and oxidize the nano-diamond first, and the pretreatment method is the same as that of the above-mentioned embodiment 1;

[0053] 2) Take 100g of purified and mixed-acid oxidation-treated nano-diamonds, add them to 1000ml of thionyl chloride, sonicate in a 200kHz, 500W ultrasonic instrument for 36h, reflux at 80°C for 72h, and then centrifuge at 6500rpm for 20min. Thionyl chloride was separated, washed with tetrahydrofuran, and vacuum-dried at room temperature for 48 hours;

[0054] 3) Take 35g of nano-diamonds containing acid chloride groups on the surface prepared in the previous step, and 380g of 1,3-propanediamine, and add them to 1200ml of N,N'-dimethylformamide respectively, under nitrogen protection, in After ultrasonication for 30h in a 200kHz, 500W ultrasonic instrumen...

Embodiment 3

[0062] The content of a kind of hydroxyl group is about 0.006% and the terminal group is the nano-diamond derivative of hydroxyl group, and its specific preparation method is as follows:

[0063] 1) Purify and oxidize the nano-diamond first, and the pretreatment method is the same as that of the above-mentioned embodiment 1;

[0064] 2) Take 100g of purified and mixed-acid oxidation-treated nano-diamonds, add them to 1000ml of thionyl chloride, sonicate in a 200kHz, 500W ultrasonic instrument for 36h, reflux at 80°C for 72h, and then centrifuge at 6500rpm for 20min. Thionyl chloride was separated, washed with tetrahydrofuran, and vacuum-dried at room temperature for 48 hours;

[0065] 3) Take 35g of nano-diamonds containing acid chloride groups on the surface prepared in the previous step, and 380g of 1,3-propanediamine, and add them to 1200ml of N,N'-dimethylformamide respectively, under nitrogen protection, in After ultrasonication for 30h in a 200kHz, 500W ultrasonic instr...

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PUM

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Abstract

The invention provides a nanodiamond derivative having hydroxy groups as terminal groups, and a preparation method and a use thereof, and belongs to the nanomaterial field. The preparation method comprises the following steps: 1, reacting nanodiamond subjected to purification and mixed acid oxidation treatment with thionyl chloride; 2, respectively carrying out a nucleophilic substitution reaction of a substance obtained in step 1 by a diamine compound and trichlorotriazine; 3, respectively carrying out the nucleophilic substitution reaction of a substance obtained in step 2 by a dibasic alcohol compound and trichlorotriazine; and 4, carrying out an iteration reaction of a substance obtained in step 3, the dibasic alcohol compound and trichlorotriazine to obtain the nanodiamond derivative having hydroxy groups as terminal groups, wherein the content of the hydroxy content in the nanodiamond derivative having hydroxy groups as terminal groups is about 0.001-0.01%. The nanodiamond derivative having hydroxy groups as terminal groups has good dissolvability in a water and parts of polar organic solvents, so the stable dispersion of nanodiamond is realized; the preparation conditions of the derivative can be easily satisfied, and the above raw materials are easy to obtain; and the derivative has the advantages of stable structure, good dispersity and stability in water and parts of polar organic solvents, high technological content, strong innovation and good application prospect.

Description

technical field [0001] The invention relates to a nano-diamond derivative, in particular to a nano-diamond derivative whose end group is a hydroxyl group, as well as a preparation method and application of the derivative, and belongs to the field of nanometer materials. Background technique [0002] The product nano-diamond has both the quantum size effect and surface effect of nano-materials, as well as the high hardness and wear resistance of diamond itself, and is of 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 agglomer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/44C09C3/08C10M125/02C10N30/06
Inventor 浣石柯刚谭湘倩
Owner 浣石
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