Manufacturer Direct Sale High Carbon Low Sulphur Graphitized Petroleum Coke GPC
Manufacturer direct sale high carbon low sulphur Graphitized Petroleum Coke GPC for metallurgy and foundry
At present, chemical and electrolytic methods are mostly used to prepare expandable graphite. Chemical method is to natural flake graphite impregnated in 100-105 ℃ of nitric acid and 98% of the mixture of sulfuric acid, reaction of 1-3 hours, then washed to PH for 3-6. Under 60-100 ℃ drying, again in 900-1000 ℃ under inflation processing, produce vermicular graphite expansion.
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The downside of this approach is in 100-105 ℃, the mixture of sulfuric acid and nitric acid is easy to produce the harmful gas such as acid mist, and the operating risk and the method, the expanded graphite containing 2-3% of sulfur. In order to overcome the shortcomings of the above methods, an electrolytic method named cn-1068152 was developed, in which the natural flake graphite was loaded into an electrolytic cell containing sulfuric acid, and the concentration of sulfuric acid was 90-98%.
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The process of anodic oxidation and cathodic reduction was carried out repeatedly in the electrolytic cell. (the dc current was 300A, the current density was 20-50ma /cm2, and the tank voltage was 2.5-6v). Then, expandable graphite was prepared by washing and drying. The deficiency of this method is the high sulfur content, that is, the sulfur content is 2-2.65%. It consumes a lot of electricity.
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This is the purpose of the present invention implementation method of the invention includes a, soaked the flake graphite oxide in 45 to 60 ℃ concentrated sulfuric acid (concentration of 90% to 98%, the dosage of graphite parts by weight of 2.5 to 5 times), stir well, add soluble lead to the water under stirring constantly two sulfate (dose to graphite parts by weight of 0.1 to 0.23 times), the reaction time about 0.5 3 hours, the reaction temperature for 45 to 60 ℃, acid graphite was prepared.
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B after oxidation desulfurization acid graphite centrifugal acid (sulfate acid amount to join in parts by weight of 0.6 to 0.9 times) after placement nitrate (concentration of 65% to 68%, the dosage of graphite parts by weight of 0.5 to 1.1 times) and oxalic acid (dosage used graphite parts by weight of 0.02 to 0.07 times) mixture, stir well, static reaction 2-6 hours, the reaction temperature is 25 and 30 ℃, graphite centrifugal acid after reaction, wash with water until the PH after 4 to 7, centrifugal dryer, c, puffed after desulfurization of graphite at 40 to 60 ℃ temperature is dry, Moisture content control in 0.5% - 1% weight number, the last expansion under the 900-950 ℃.
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The recovered sulfuric acid after oxidation can be recycled for many times, that is, sulfuric acid is added to the recovered sulfuric acid (the concentration is 90%-98%, and the dosage is 0.1-0.4 times of the weight of the original sulfuric acid) and ammonium perdisulfate (the dosage is 0.1-0.15 times of the weight of graphite). In addition, the dilute acid solution produced by desulfurization washing is added with ammonium bicarbonate (the amount is 0.5-1.2 times the weight of graphite) to produce a mixture of ammonium sulfate and ammonium nitrate.
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Compared with the existing technology, the invention has the following significant advantages: first, the expandable graphite produced in this production process has a low sulfur content. Secondly, it reduces environmental pollution and energy consumption. In addition, this method is simple, easy to hold, stable product quality.
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Implementation of 1 to 10 grams of graphite soaking in the temperature of 50 ℃, weight is 40 grams of sulphuric acid concentration (98%) in the solution, mixing evenly, then under stirring constantly add 1.5 grams of solid two ammonium sulfate. 40 minutes, the reaction temperature is 50 ℃. After the reaction, the will of the acidic graphite centrifugal desulfurization, remove after 33 grams of sulfuric acid and then add 10 grams of nitric acid concentration (65%) and 0.5 grams of oxalic acid mixture, stir well, static reaction 3 hours, the reaction temperature is 25 ℃, the reaction after graphite centrifugal acid, wash with water until the PH value of 6, centrifugal dry, and dry under 60 ℃, until the water content is 0.8% of the graphite parts by weight, then through the high temperature of 950 ℃ 50 seconds, can produce the expansion volume of 220 ml/g, the sulfur content of 0.8% can be expanded graphite.
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In order to reduce the cost, the sulfur acid recovered after oxidation can be recycled for many times, that is, adding sulfuric acid (the concentration is 90%-98%, the dosage is 0.1-0.4 times of the weight of the original sulfuric acid) and ammonium perdisulfate (the dosage is 0.1-0.15 times of the weight of graphite) into the recovered sulfur acid solution. In addition, the dilute acid solution produced by desulfurization washing is added with ammonium bicarbonate (the amount is 0.5-1.2 times the weight of graphite) to produce a mixture of ammonium sulfate and ammonium nitrate.
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