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Preparation method of graphene

A technology of graphene and graphene dispersion liquid, which is applied in the field of graphene preparation, can solve the problems of low graphene yield and achieve the effects of excellent product performance, improved preparation efficiency, and simple process

Active Publication Date: 2014-10-01
广州市尤特新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the third method has also been discussed above, mainly through the Hummers method or the improved Hummers method to prepare GO, and then reduce GO with sodium borohydride to obtain graphene oxide. The yield of graphene obtained by this method is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 1. Add 1g of 500-mesh granular natural graphite and 0.5g of sodium nitrate into a 250mL three-necked flask under ice-water bath conditions. Then slowly add 24mL concentrated sulfuric acid (mass concentration: 98%) into the there-necked flask and stir thoroughly to keep the reaction temperature of the system at about 0°C. First, use an ultrasonic cell pulverizer with a working frequency of 20kHz and an ultrasonic power of 800w for 15 minutes, and then use Ultrasonic treatment with an ultrasonic cleaner with a working frequency of 20kHz and an ultrasonic power of 120w for 30 minutes, and finally ultrasonic treatment with an ultrasonic cell pulverizer with a working frequency of 20kHz and an ultrasonic power of 800w for 15 minutes. During the ultrasonic treatment, an ice bath must be used to keep the system temperature at about 0 ℃, fully stirred for 2~3h after ultrasonic treatment.

[0054] 2. Add 3.0 g of potassium permanganate into a three-necked flask, keep the tempera...

Embodiment 2

[0064] 1. Add 1g of 500-mesh granular natural graphite and 0.5g of sodium nitrate into a 250mL three-necked flask under ice-water bath conditions. Then slowly add 24mL concentrated sulfuric acid (mass concentration: 98%) into the there-necked flask and stir well to keep the reaction temperature of the system at about 0°C. First, use an ultrasonic cleaner with a working frequency of 20kHz and an ultrasonic power of 120w for 15 minutes, and then use a working Ultrasonic treatment with a frequency of 20kHz and an ultrasonic power of 800w for 30 minutes, and finally ultrasonic treatment with an ultrasonic cleaner with a working frequency of 20kHz and an ultrasonic power of 120w for 15 minutes. During the ultrasonic treatment, an ice bath must be used to keep the system temperature at about 0°C , fully stirred for 2~3h after ultrasonic treatment.

[0065] 2. Add 3.0 g of potassium permanganate into a three-necked flask, keep the temperature of the reaction system below 10°C, keep t...

Embodiment 3

[0074] 1. Add 1g of 500-mesh granular natural graphite and 0.5g of sodium nitrate into a 250mL three-necked flask under ice-water bath conditions. Then slowly add 24mL of concentrated sulfuric acid (mass concentration: 98%) into the three-necked flask and stir thoroughly, keeping the reaction temperature of the system not higher than 5°C, and fully react for 3 hours.

[0075] 2. Add 3.0g of potassium permanganate into the three-necked flask, keep the temperature of the reaction system at 20-30°C, and keep stirring for 3 hours.

[0076] 3. Add 500ml of crushed ice cubes, and add 20ml of hydrogen peroxide solution with a mass concentration of 3% drop by drop until the gas completely escapes.

[0077] 4. Add 20ml of hydrochloric acid with a mass concentration of 10%, react fully, and repeat centrifugation with deionized water not higher than 10°C until the pH of the supernatant is neutral.

[0078] 5. The obtained precipitate is ultrasonically treated with an ultrasonic pulveriz...

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Abstract

The invention discloses a preparation method of graphene. The preparation method comprises the following steps: (1) reacting graphite powder, sodium nitrate and concentrated sulfuric acid at -5 DEG C to 0 DEG C; (2) adding potassium permanganate, and reacting to prepare graphite suspension liquid; (3) adding dilute sulphuric acid and ultrasonically processing; (4) adding de-ionized water; (5) adding a hydrogen peroxide solution till all gas escapes; (6) adding hydrochloric acid, fully reacting to obtain a product, and washing the product by using the de-ionized water; (7) fully dispersing deposits in the de-ionized water; and (8) adding oxalic acid powder, and reacting to remove excessive oxalic acid. According to the preparation method, a physical process is combined with a chemical process and the intercalation and stripping degree of graphite oxide is increased, so that the preparation efficiency of graphene is improved and the yield is increased by 25%-30% in comparison with that of an oxidation-reduction process in the prior art; in addition, the preparation method achieves high-yield preparation of high-quality graphene, has the characteristics of simple process and the like and is suitable for large-scale production of multi-layer graphene, and the product performance is excellent.

Description

technical field [0001] The invention relates to a preparation method of graphene. Background technique [0002] In addition to three-dimensional layered graphite, scientists have discovered that the carbon family also has zero-dimensional fullerenes, one-dimensional carbon nanotubes, and whether two-dimensional carbon materials can exist stably at room temperature has always been a mystery. As early as many years ago, famous physicists Peierls and Landau proposed theoretically that strictly two-dimensional crystals cannot exist due to their thermodynamic instability. In 1966, the Mermin-Wagner theory of Mermin and Wagner pointed out that long wavelength fluctuations would also destroy long-range ordered two-dimensional crystals. At this time, two-dimensional carbon materials are considered to be only a theoretical model, but this has not hindered people's theoretical and experimental exploration of two-dimensional carbon materials. Scientists have tried to obtain stable sin...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 徐国华沈艳斌朱鑫
Owner 广州市尤特新材料有限公司
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