Method for preparing microwave absorbing nano-material

Method for preparing microwave absorbing nano-material

  • CN 104,531,061 A
  • Filed: 01/12/2015
  • Published: 04/22/2015
  • Est. Priority Date: 01/12/2015
  • Status: Active Application
First Claim
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1. a preparation method for nano wave-absorbing material, is characterized in that, its step is as follows:

  • Step one, made by graphite and be of a size of 50-200 order and obtain Graphite Powder 99, being added to massfraction is afterwards in the hydrochloric acid soln of 35%, stirs 30min, adopts deionized water repeatedly to rinse afterwards and makes pH value be neutral, dry stand-by;

    Stand-by Graphite Powder 99, Potassium Persulphate and P will be dried above 2o 5add in the vitriol oil, form mixture, the pH value of the mixture formed is 1.5, and this mixture is stirred 1-2h at 60 DEG C, then 2-4h is stirred with at the ramp to 80 of 5 DEG C/min DEG C, finally being warming up to 87 DEG C with 2 DEG C/min stirs skewer 1-2h, then adopts this mixture of distilled water diluting, the pH value of this mixture is diluted to 3.6, distilled water is adopted to filter after placing 36h, make mixture pH value be 6-7, after carry out drying at room temperature, described Graphite Powder 99, Potassium Persulphate, P 2o 5be 1-3;



    5-10 with the mass ratio of the vitriol oil;

    Joined in concentrated nitric acid by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and concentrated nitric acid is 1-4;

    50-100, and after stirring, at-8 DEG C, first time adds KMnO 4, stir 30min, at being cooled to-12 DEG C afterwards, second time adds KMnO 4, stir 30min, at being finally cooled to-15 DEG C, third time adds KMnO 4, stir 20min, obtain the graphite mixture of preoxidation, described first time adds KMnO 4, second time adds KMnO 4kMnO is added with third time 4mass ratio be 1;


    3, described dried mixture and total KMnO 4ratio be 1-2;


    After the graphite mixture obtaining preoxidation is filtered also drying, be positioned in retort furnace and carry out heat treated, heat treated temperature, for process 10-20s at 1100 DEG C, processes 13-20s at 1150 DEG C, processes 20-30s, obtain expanded graphite at 1180 DEG C;

    Step 2, puts into insulation can by expanded graphite made for step one and is warmed up to 40 DEG C, reaction 3h, subsequently, add the first distilled water with the consistent amount of graphite mixture volume of preoxidation, then react 2.5h, by insulation can temperature to 40 DEG C, again add after-fractionating water and H 2o 2reaction 10-60min, the amount of described after-fractionating water is 1-1.5 times of the first distilled water, after-fractionating water and H 2o 2volume ratio be 4-20;

    1, carry out centrifugation 10min, rotating speed 8000-10000r/min after reaction terminates, centrifugation after product hydrochloric acid soln washs, the volume of this hydrochloric acid soln is 10-50 times of centrifugation after product volume, and finally dialysis obtains graphite oxide in 7-8 days;

    Add N-hydroxysuccinimide after graphite oxide being adopted methyl-sulphoxide ultrasonic dissolution and make surface treatment agent by oneself and stir 2h at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide. Step 3, the ethylene glycol ultrasonic disperse putting into 500ml after surface-treated graphite oxide 1-2g step 2 obtained carries out frost drying at-10-30 DEG C with 1-10g polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer in the lump forms uniform first dispersion liquid;

    Simultaneously by 4-15g by FeCl 36H 2o, FeCl 24H 2the mixture of O and acetyl acetone iron composition, 6 ~ 25g polyvinylpyrrolidone and 10 ~ 50g NH 4ac is dissolved in the ethylene glycol of 500-1000mL and forms the second dispersion liquid, by the first dispersion liquid and the second dispersion liquid mix and blend, and regulates with ammoniacal liquor, makes it to become the settled solution that pH value is 8-10, described FeCl 36H 2o, FeCl 24H 2the mass ratio of O and acetyl acetone iron is 1;



    Step 4, the settled solution that 100ml step 3 obtains is put into reactor, after sealing, be heated to 150 DEG C, insulation 2h, 200 DEG C are warming up to afterwards with the temperature rise rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the temperature rise rate of 3-6 DEG C/min, insulation 3h, then 200 DEG C of insulation 2h are cooled to the cooling rate of 5-7 DEG C/min, finally be warming up to 235 DEG C with the temperature rise rate of 3-6 DEG C/min again, insulation 7h, after question response completes, reactor is taken out, make it cool to room temperature, described cooling rate is 3-6 DEG C/min, by the black powder centrifugation 10min of gained, rotating speed 8000-10000r/min, dehydrated alcohol and deionized water is adopted respectively to wash three times, at 50-70 DEG C of vacuum-drying 24h, obtain the first product,Be added in the solution of Witco 1298 Soft Acid by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and Witco 1298 Soft Acid is 1-1.5;


    3g ammonium persulphate is dissolved in 80-120ml distilled water, is slowly added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, uses distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain nano wave-absorbing material.

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