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-con

Method used

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

Examples

Experimental program
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Example Embodiment

[0014] Example 1: Purify nano-diamond soot according to the following steps

[0015] (1) Removal of metal impurities: In a 50L reactor, add 25.0kg of 20% nitric acid, add 5.00kg of nano-diamond ash under stirring, and heat to 70 o C, stirring for 48h, cooling to room temperature, vacuum filtration, and washing with deionized water to neutrality, the solid matter in 80 o C is dried under vacuum to obtain 4.22kg of purified product once; the yield is 84.4%;

[0016] (2) Removal of graphite carbon impurities: In a 50L reactor, put 10.0kg of 98% sulfuric acid with a mass concentration of 98%, add 3.00kg of the purified product under stirring, and heat up to 250 under vacuum. o C, 16.0kg of 70% perchloric acid with a mass concentration of 70% is added dropwise, and the temperature in the kettle is controlled to 200 during the dropping process o C, after 8 hours of dripping, then 250 o C keep warm for 1 hour, cool to 40 o C. Pour into 50L of deionized water, filter, and fully wash with dei...

Example Embodiment

[0018] Example 2: Purify nano-diamond soot according to the following steps

[0019] (1) Removal of metal impurities: In a 50L reactor, add 40.0kg of 5% nitric acid, under stirring, add 5.00kg of nano-diamond soot, and heat to 95 o C, stirring for 1h, after cooling to room temperature, vacuum filtration, and fully wash with deionized water to neutral, the solid matter at 80 o C is dried under vacuum to obtain 4.02kg of purified product once; the yield is 80.4%;

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

Example Embodiment

[0022] Example 3: Purify nano-diamond soot according to the following steps

[0023] (1) Removal of metal impurities: In a 50L reactor, add 20.0kg of 50% nitric acid, under stirring, add 4.00kg of nano-diamond soot, and the temperature is controlled to 10 o C, stir for 24h, after cooling to room temperature, vacuum filter, and fully wash with deionized water to neutral, the solid matter in 80 o C is dried under vacuum to obtain 3.66kg of purified product; the yield is 91.5%;

[0024] (2) Removal of graphite carbon impurities: Put 40kg of 90% sulfuric acid with a mass concentration of 90% in a 50L reactor, add 2.00kg of primary purified product under stirring, and raise the temperature to 180 under vacuum. o C, 15kg of 40% perchloric acid is added dropwise, and the temperature in the kettle is controlled 170-210 during the dropping process o C, then 180 o C keep warm for 10 hours and cool to 40 o C. Pour into 100L of deionized water, filter, and fully wash with deionized water until t...

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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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