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Purification method of nano diamond ash material

A technology of nano-diamond and purification method, which is applied in the field of joint removal of graphite carbon, metal oxide and silicon dioxide impurities. The effect of simple process, low equipment requirements and high product purity

Inactive Publication Date: 2012-08-01
江苏金海丰硬质材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of its method is to use concentrated sulfuric acid + concentrated nitric acid, at 230 o When reacting at C, the decomposition reaction of concentrated nitric acid is difficult to control, and at the same time, due to the oxidizing properties of the two high-concentration acids themselves, the removal effect for metal oxides will not be ideal, and the process requirements are difficult; Calcium impurities, after hydrofluoric acid treatment, easily form insoluble calcium fluoride insoluble matter, which becomes more difficult to remove

Method used

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  • Purification method of nano diamond ash material
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  • Purification method of nano diamond ash material

Examples

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Effect test

Embodiment 1

[0014] Embodiment 1: purify nano-diamond dust material according to the following steps

[0015] (1) Removal of metal impurities: In a 50L reaction kettle, add 25.0kg of 20% nitric acid, add 5.00kg of nano-diamond ash material under stirring, and heat up to 70 o C, stirred for 48h, cooled to room temperature, vacuum filtered, and fully washed with deionized water to neutrality, the solid matter at 80 o C is vacuum-dried to obtain 4.22kg of a purified product; yield 84.4%;

[0016] (2) Removal of graphite carbon impurities: In a 50L reactor, put 10.0kg of sulfuric acid with a mass concentration of 98%, add 3.00kg of a purified product under stirring, and heat up to 250 under vacuum o C, dropwise add 16.0kg of mass concentration 70% perchloric acid, control the temperature in the kettle to 200°C during the dropwise addition process o C, the dropwise addition was completed in 8 hours, and then 250 o C for 1 hour, cool to 40 o C, poured into 50L deionized water, filtered, and ...

Embodiment 2

[0018] Embodiment 2: purify nano-diamond dust material according to the following steps

[0019] (1) Removal of metal impurities: In a 50L reaction kettle, add 40.0kg of 5% nitric acid, add 5.00kg of nano-diamond ash material under stirring, and heat up to 95 o C, stirred for 1h, cooled to room temperature, vacuum filtered, and fully washed with deionized water to neutrality, the solid matter at 80 o C is vacuum-dried to obtain 4.02kg of a purified product; yield 80.4%;

[0020] (2) Removal of graphite carbon impurities: In a 50L reactor, put 15.0kg of sulfuric acid with a mass concentration of 94%, add 1.00kg of a purified product under stirring, and heat up to 180 under vacuum o C, dropwise add 55% perchloric acid with a mass concentration of 20.0kg, and control the temperature in the kettle to 180-230°C during the dropwise addition process o C, the dropwise addition was completed in 7 hours, and then 210 o C for 5 hours, cool to 40 o C, poured into 60L deionized water, ...

Embodiment 3

[0022] Embodiment 3: purify nano-diamond dust material according to the following steps

[0023] (1) Removal of metal impurities: In a 50L reactor, add 20.0kg of 50% nitric acid, add 4.00kg of nano-diamond ash material under stirring, and control the temperature for 10 o C, stirred for 24h, cooled to room temperature, vacuum filtered, and fully washed with deionized water to neutrality, the solid matter at 80 o C is vacuum-dried to obtain 3.66kg of a purified product; yield 91.5%;

[0024] (2) Removal of graphite carbon impurities: In a 50L reactor, put 40kg of sulfuric acid with a mass concentration of 90%, add 2.00kg of a purified product under stirring, and heat up to 180 under vacuum o C, dropwise add 15kg of 40% perchloric acid in mass concentration, and control the temperature in the kettle to 170-210°C during the dropwise addition process o C, then 180 o C for 10 hours, cool to 40 o C, poured into 100L deionized water, filtered, and fully washed with deionized water...

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Abstract

The invention discloses a purification method of a nano diamond ash material. The method adopts a three-step method to remove impurities in nano diamond detonated ash and comprises the following steps of: step 1, utilizing nitric acid or hydrochloric acid to remove impurities including metal oxides or metal salts; step 2, utilizing a concentrated sulfuric acid and perchloric acid united oxidization method to remove graphite carbon components in nano diamond; and step 3, utilizing hydrofluoric acid to remove silicon oxide. The invention provides a production method of the high-purity nano diamond, which has the advantages of simple process, low equipment requirements and high product purity; and the produced nano diamond can completely meet the requirements of relevant fields, particularly the application of fields including ultra-precise polishing, high-grade running-in (lubricating) oil, wear-resisting material additives, wear-resisting surface composite plating and the like.

Description

technical field [0001] The invention relates to a method for purifying nano-diamond ashes, in particular to a combined removal method for graphite carbon, metal oxides and silicon dioxide impurities in nano-diamond ashes prepared by explosive detonation. Background technique [0002] Synthesis of nano-diamond by detonation method is a new technology developed in the past ten years. The average diameter of the diamond particles synthesized by the detonation method is between 4-8nm, which has the dual characteristics of diamond and nano particles. Fields have a wide range of uses. [0003] The diamond-like carbon-containing detonation ash mixture prepared by explosive detonation contains various impurities such as graphite, silicon dioxide, and metal oxides, which must be removed. The removal methods of graphitic carbon impurities currently reported include strong acid oxidation, high temperature air oxidation and other technologies. (1) CN1385366A discloses to use pota...

Claims

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Application Information

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IPC IPC(8): C01B31/06B82Y40/00C01B32/28
Inventor 陈守文解立新胡朝霞
Owner 江苏金海丰硬质材料科技有限公司
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