Method for preparing expandable graphite by using ozone

An expanded graphite and ozone technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of unfavorable acid recycling, reduction of oxidant consumption, heavy metal ion pollution, etc. The effect of environmental pollution and simple equipment and process

Inactive Publication Date: 2012-10-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical oxidation method is to oxidize graphite with a mixed solution of strong oxidizing acids such as concentrated sulfuric acid, concentrated nitric acid, perchloric acid and strong oxidants such as potassium dichromate, potassium perchlorate, potassium permanganate, peroxide, etc. The method is simple, But acid consumption is big, is unfavorable for the recycling of acid solution, and may cause the pollution of heavy metal ion in the production process, relevant Chinese patent application publication number has: CN1462724A, CN11884060A, CN1613757A, CN101327926A, CN101786618A, CN101100297A etc.
The electrochemical method is to use natural flake graphite and auxiliary anode together to form an anode chamber, intercalation agents such as sulfuric acid solution and ammonium nitrate solution as electrolyte, and direct current or pulse current to anodize graphite. Compared with chemical methods, this method has a The amount of oxidizing agent is greatly reduced, but the equipment is more complicated. The relevant Chinese patent application publication numbers are: CNl1117021A, CN1113215A, CNl102444A, CN1096827A, CN1029693C, CN1030535C, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of expandable graphite, put 10 grams of 50 mesh natural flake graphite in a 500ml measuring cylinder; add 200ml of concentrated sulfuric acid with a mass fraction of 98% to form a graphite intercalant mixture; Put the pipette into the mixed solution of graphite intercalation agent for oxidative intercalation, continue mechanical stirring at about 25°C, react for 30 hours, suction filter and wash with water until the pH of the filtrate is 6-7; dry in an oven at 50°C After 48 hours, expandable graphite was obtained. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a resistance furnace at 950°C is 240 ml / g. Among them, the ozone generator used is OZ-3G type, industrial oxygen gas source, oxygen flow rate is 5 liters / hour, and the ozone concentration adjustment knob is adjusted to 100%.

Embodiment 2

[0022] The preparation method of expandable graphite is that 5 grams of 50 mesh natural flake graphite is placed in a 500ml graduated cylinder; 180ml of concentrated sulfuric acid with a mass fraction of 98% and 20ml of nitric acid with a mass fraction of 65% are added to form a mixed solution of graphite intercalation agent; Through an ozone generator, directly pass ozone into the graphite intercalation agent mixture through a glass straw for oxidative intercalation, and continuously mechanically stir at about 15°C. After reacting for 21 hours, suction filter and wash with water until the pH of the filtrate is 6-7 ; Dry in an oven at 50° C. for 48 hours to obtain expandable graphite. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a 900°C resistance furnace is 208 ml / g. Among them, the ozone generator used is OZ-3G type, industrial oxygen gas source, oxygen flow rate is 5 liters / hour, and the ozone concentration adjustm...

Embodiment 3

[0024] The preparation method of expandable graphite is that 5 grams of 50 mesh natural flake graphite is placed in a 500ml graduated cylinder; 180ml of concentrated sulfuric acid with a mass fraction of 98% and 20ml of formic acid with a mass fraction of 88% are added to form a mixed solution of graphite intercalation agent; Through an ozone generator, directly pass ozone through a glass straw into the graphite intercalation agent mixture for oxidative intercalation, continue mechanical stirring at about 15°C, react for 22 hours, suction filter and wash with water until the pH of the filtrate is 6-7 ; Dry in an oven at 50° C. for 48 hours to obtain expandable graphite. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a 900°C resistance furnace is 216 ml / g. Among them, the ozone generator used is OZ-3G type, industrial oxygen gas source, oxygen flow rate is 5 liters / hour, and the ozone concentration adjustment knob is adj...

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Abstract

The invention relates to a method for preparing expandable graphite by using ozone. Concentrated sulfuric acid, fuming nitric acid, perchloric acid or mixed acid is adopted to oxidize crystalline flake graphite, together with oxidant, the temperature of the oxidation reaction is 5-50 DEG C, the oxidation reaction lasts for 30 min-100 hours, and then the pH value is adjusted to be 6-7 through suction filtration and water scrubbing, the oxidized graphite is dried for 10-72 hours at the temperature of 40-60 DEG C, and the expandable graphite is obtained. The mixed acid at least contains concentrated sulfuric acid, fuming nitric acid or perchloric acid; and the oxidant is ozone or mixed oxidant containing ozone. The method provided by the invention has the following advantages: the oxidative products of ozone are oxygen and water, no other residual materials are produced, and the secondary pollution is not caused; the ozone is easy to prepare, and the equipment and technique are simple; and the source of ozone is easy to obtain and is not limited by transportation conditions. Ozone is adopted to oxidize the graphite, so that the environmental protection is reduced, and the instability and insecurity of peroxides are also avoided, and meanwhile, the recycling of intercalation solution is facilitated.

Description

technical field [0001] The invention relates to a method for preparing a graphite material, in particular to a method for preparing expandable graphite by using ozone. Background technique [0002] Expandable graphite is a new type of compound with interlayer intercalation formed by natural flake graphite through oxidative intercalation reaction to insert heterogeneous atoms, molecules or ions between graphite flakes. When the expandable graphite is subjected to high temperature, the interlayer intercalation material is rapidly vaporized by the high heat, and the formed gas generates a huge stretching tension on the graphite sheet, so that the expandable graphite expands, and the expansion multiple is as high as tens to hundreds of times. The generated charcoal layer has excellent oxidation resistance and high temperature resistance, which can protect the material under the charcoal layer and achieve the purpose of flame retardancy and fire prevention. Compared with traditi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/205
Inventor 刘定福
Owner SOUTH CHINA UNIV OF TECH
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