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Method for purifying nano-diamond

A nano-diamond and purification method technology, which is applied in the field of nano-diamond purification, can solve the problems of complicated nano-diamond removal routes and low removal efficiency, and achieve the effects of avoiding metal ion precipitation, improving removal efficiency, and saving consumption

Inactive Publication Date: 2018-09-28
成都天成鑫钻纳米科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a method for purifying nano-diamonds in view of the problems of complex removal routes and low removal efficiency of the existing nano-diamonds

Method used

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  • Method for purifying nano-diamond

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A method for purifying nano-diamonds, comprising the following steps:

[0036] (1) Adding the nano-diamond black powder to a mass concentration of 96% H 2 SO 4 solution and a mass concentration of 90% H 3 PO 4 solution mixture, heated and stirred for 30min, then added KMnO 4, the temperature of the control system is 75°C, and the reaction is 3h, wherein, nano-diamond black powder, mixed solution, KMnO 4 The mass ratio is 1:4:0.6, H 2 SO 4 solution and H 3 PO 4 The volume ratio of the solution is 1:1;

[0037] (2) the solution after step (1) reaction is cooled to room temperature, then adopts ceramic membrane filter to filter, wash with water, obtain the nano-diamond after rough extraction;

[0038] (3) Adding the nano-diamond after rough extraction in step (2) into a NaOH solution with a concentration of 0.6mol / L and stirring for 3h;

[0039] (4) The solution after the reaction in step (3) is filtered by a ceramic membrane filter, washed with water, and dried ...

Embodiment 2

[0043] A method for purifying nano-diamonds, comprising the following steps:

[0044] (1) Adding the nano-diamond black powder to a mass concentration of 90% H 2 SO 4 solution and a mass concentration of 85% H 3 PO 4 solution mixture, heated and stirred for 45min, then added KMnO 4 , the temperature of the control system is 85°C, and the reaction is 2.5h, wherein, nano-diamond black powder, mixed solution, KMnO 4 The mass ratio is 1:6:0.8, H 2 SO 4 solution and H 3 PO 4 The volume ratio of the solution is 2:1;

[0045] (2) the solution after step (1) reaction is cooled to room temperature, then adopts ceramic membrane filter to filter, wash with water, obtain the nano-diamond after rough extraction;

[0046] (3) Adding the nano-diamond after rough extraction in step (2) into a KOH solution with a concentration of 1mol / L and stirring for 2.5h;

[0047] (4) The solution after the reaction in step (3) is filtered by a ceramic membrane filter, washed with water, and drie...

Embodiment 3

[0051] A method for purifying nano-diamonds, comprising the following steps:

[0052] (1) Adding the nano-diamond black powder to a mass concentration of 82% H 2 SO 4 solution and a mass concentration of 81% H 3 PO 4 solution mixture, heated and stirred for 60min, then added KMnO 4 , the temperature of the control system is 100°C, and the reaction is 2h, wherein, nano-diamond black powder, mixed solution, KMnO 4 The mass ratio is 1:9:1, H 2 SO 4 solution and H 3 PO 4 The volume ratio of the solution is 3:1;

[0053] (2) the solution after step (1) reaction is cooled to room temperature, then adopts ceramic membrane filter to filter, wash with water, obtain the nano-diamond after rough extraction;

[0054] (3) Adding the nano-diamond after rough extraction in step (2) into a NaOH solution with a concentration of 2mol / L and stirring for 1h;

[0055] (4) The solution after the reaction in step (3) is filtered by a ceramic membrane filter, washed with water, and dried at...

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Abstract

The invention discloses a method for purifying nano-diamond. The method comprises the following steps: (1) adding nano-diamond black powder into a mixed liquor of a H2SO4 solution and a H3PO4 solution, heating and stirring, adding KMnO4, controlling the system temperature at 70-100 DEG C, and reacting for 2-3h; (2) cooling the solution after the reaction to room temperature, filtering, and washingwith water to obtain coarsely extracted nano-diamond; (3) adding the crudely extracted nano-diamond to an alkaline solution for stirring and reacting; (4) filtering the reacted solution, washing withwater, and drying to obtain pure nano-diamond. According to the invention, metal ions formed after removal of metal impurities are combined with phosphate anions to form a coordination compound, themetal ions precipitation can be avoided, so that the removal of the metal impurities and graphite can be simultaneously performed, the route is simplified, and the impurity removal efficiency is improved, and concentrated hot phosphoric acid can corrode silicon dioxide to achieve the purpose of preliminary removal of Si and improve the subsequent Si removal efficiency.

Description

technical field [0001] The invention belongs to the technical field of diamond purification, and in particular relates to a method for purifying nano-diamonds. Background technique [0002] The detonation method is a novel method for preparing nanomaterials. In recent decades, many researchers have used the detonation method to prepare nanomaterials such as diamond, graphite, and boron nitride under high temperature and high pressure conditions. Nanodiamonds synthesized by the detonation method usually contain impurities such as graphite, metal impurities (mainly Fe) and Si, which must be removed. [0003] At present, the impurity removal process of nano-diamond is mainly the "three removal" process: (1) acid removes alloy impurities to convert metal into metal ions; (2) strong oxidant removes graphite to convert C into CO 2 Gas; (3) Alkali fusion of Si impurities. The oxidation process uses perchloric acid, sulfuric acid and nitric acid. Among them, perchloric acid will i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/28
Inventor 刘欢锐邓文才何昱江
Owner 成都天成鑫钻纳米科技股份有限公司
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