Method for preparing layered nano carbon material by coal solvent heat treatment
A technology of layered nano and carbon materials, applied in the direction of nano carbon
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Embodiment 1
[0065] Ash-free lignite is selected as the raw material, and the massive raw coal is crushed by mechanical crushing, and then sieved to control the particle size below 0.15mm. The pulverized raw coal was treated with 25 times deionized water in an ultrasonic cleaner (20 kHz) for 30 minutes, filtered and then dried in a drying machine at 110° C. until the water content was lower than 5%. Coal powder is mixed with benzyl alcohol-benzyl ether solvent to form coal slurry, which is then heated in a closed high-pressure reactor.
[0066] The molar ratio of the benzyl alcohol-benzyl ether solvent and the composition of the coal slurry are shown in Table 3. 400ml of coal slurry was injected into a 1L stainless steel reaction kettle, and the air was exhausted with nitrogen after sealing. The temperature of the coal slurry is raised to 380°C, the stirring rate is 300r / min, and the treatment time is 2.5h.
[0067]The solvent and low boilers are separated off after the liquefaction proce...
Embodiment 2
[0073] The ashless lignite is used as raw material, and the lump coal is crushed by mechanical crushing, and then sieved to control the particle size below 0.15mm. The pulverized raw coal was treated with 25 times deionized water in an ultrasonic cleaner (20kHz) for 30min, filtered and dried at 110°C until the moisture content was less than 5%; coal powder was mixed with benzyl alcohol-benzyl ether solvent to form coal slurry , and then heat-treated in a closed autoclave.
[0074] The molar ratio of benzyl alcohol-benzyl ether solvent was 1:1, and the mass ratio of solvent to coal powder was 4:1. 400ml of coal slurry was injected into a 1L stainless steel reactor, and the air was exhausted with nitrogen after sealing. The solvothermal treatment conditions are shown in Table 4.
[0075] The solvent and low boilers are separated off after the liquefaction process. Take 10 g of coal solvent heat treatment product, mix it with 140 ml of oxidizing agent (containing 23% nitric aci...
Embodiment 3
[0082] The ashless lignite is used as raw material, and the lump coal is crushed by mechanical crushing, and then sieved to control the particle size below 0.15mm. The pulverized raw coal was treated with 25 times deionized water in an ultrasonic cleaner (20kHz) for 30min, filtered and dried at 110°C until the moisture content was less than 5%. Coal powder is mixed with benzyl alcohol-benzyl ether solvent to form coal slurry, which is then heated in a closed autoclave.
[0083] The molar ratio of benzyl alcohol-benzyl ether solvent is 3:1, and the mass ratio of solvent to pulverized coal is 6:1. 400ml of coal slurry is injected into a 1L stainless steel reactor, and the air is exhausted with nitrogen after sealing.
[0084] The solvent and low boilers are separated off after the liquefaction process. Take 10g of coal solvothermal treatment product, mix with 140ml of oxidant, and the oxidation treatment conditions are shown in Table 5.
[0085] The oxidized product was washed...
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