A kind of preparation method of composite wave-suction material

A kind of preparation method of composite wave-suction material

  • CN 104,559,922 B
  • Filed: 01/12/2015
  • Issued: 04/06/2018
  • Est. Priority Date: 01/12/2015
  • Status: Active Grant
First Claim
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1. a kind of preparation method of composite wave-suction material, it is characterised in that its step is as follows:

  • Step 1, pre-oxidize the preparation of graphiteBy graphite powder, potassium peroxydisulfate and P2O5Adding in the concentrated sulfuric acid, form mixture, the pH value of the mixture formed is 1.5,The mixture is stirred into 1-2h at 60 DEG C, is then warming up to 5 DEG C/min speed at 80 DEG C and stirs 2-4h, finally with 2 DEG C/Min is warming up to 87 DEG C of stirring 1-2h, then using the distilled water diluting mixture, the pH value of the mixture is diluted into 3.6, putPut after 36h using distillation water filtration so that mixture ph 6-7, carry out drying at room temperature afterwards, the graphite powder, potassium peroxydisulfate,P2O5Mass ratio with the concentrated sulfuric acid is 1-3;

    1-2;

    1-2;

    5-10;

    Dried mixture is added in concentrated nitric acid and stirs 45-60min so that pH value 2-4, the dried mixingThe mass ratio of thing and concentrated nitric acid is 1-4;

    50-100, KMnO is added for the first time at -8 DEG C after stirring4, 30min is stirred, itAfter be cooled at -12 DEG C second and add KMnO4, 30min is stirred, is finally cooled at -15 DEG C and adds KMnO for the third time4, stirring20min, the graphite mixture pre-oxidized, the first time add KMnO4, second of addition KMnO4Added with third timeKMnO4Mass ratio be 1;

    2;

    3, the dried mixture and total KMnO4Ratio be 1-2;

    10-15;

    Step 2, the preparation of the graphite oxide of surface treatmentThe graphite mixture of the made pre-oxidation of step 1 is put into incubator and is warming up to 40 DEG C, reacts 3h, then, add withConsistent amount of first distilled water of graphite mixture volume of pre-oxidation, then reacts 2.5h, by incubator temperature to 40 DEG C,After-fractionating water and H are added again2O210-60min is reacted, the amount of the after-fractionating water is 1-1.5 times of the first distilled water,After-fractionating water and H2O2Volume ratio be 4-20;

    1,10min, rotating speed 9500r/min is centrifuged after terminating in reaction, fromProduct is washed with hydrochloric acid solution after heart separation, and the volume of the hydrochloric acid solution is 10-50 times of bulk product after centrifuging, finallyDialysis obtains graphite oxide in 7-8 days,Graphite oxide is put into purification liquid mixing liquid is made, carry out the oxidation stone that concussion is scattered and is filtrated to get after must purifyingInk, the purification liquid is due to the 1.72g/ml concentrated sulfuric acid and H2O2Composition, the concentrated sulfuric acid and H2O2Mass ratio be 1-2;

    2-5;

    N- hydroxysuccinimides are added after graphite oxide after purification is used into dimethyl sulfoxide ultrasonic dissolution and from control surface2h is stirred in reason agent at 35 DEG C, and product is filtered, washed, dried, that is, the graphite oxide being surface-treated;

    The ratio of graphite oxide g described in step 2, dimethyl sulfoxide ml, N- hydroxysuccinimide g and self-control surface conditioning agent gIt is worth for 0.2-0.5:

    20-25:

    2-5:

    0.1-05, the self-control surface conditioning agent is by dicyclohexylcarbodiimide, dodecyl sulphurSour sodium, kayexalate and polyacrylic acid composition, the dicyclohexylcarbodiimide, dodecyl sodium sulfate, polyphenyl secondThe mass ratio of alkene sodium sulfonate and polyacrylic acid is 1;

    1;

    2;

    3;

    Step 3, disperseAfter the graphite oxide 1-2g of surface treatment obtained by step 2 is freezed dried at -10 DEG C with 1-10g polycyclicsOxidative ethane-PPOX-PEO triblock copolymer and 1g are made up of polymethylacrylic acid and polyacrylamideMixture, the mass ratio of the polymethylacrylic acid and polyacrylamide is 1;

    1, it is put into 500ml ethylene glycol to enter in the lumpRow ultrasonic disperse, 36h is then radiated under ultraviolet irradiation and forms uniform first dispersion liquid;

    Simultaneously by 4-15g by FeCl3·

    6H2O、

    FeCl2·

    4H2O and acetyl acetone iron composition mixture, 6~25g polyethylenePyrrolidones and 10~50g NH4Ac, which is dissolved in 500-1000mL ethylene glycol, forms the second dispersion liquid, by the first dispersion liquidMix with the second dispersion liquid, and adjusted with ammoniacal liquor, make the settled solution that pH value is 8-10, the FeCl3·

    6H2O、

    FeCl2·

    4H2The mass ratio of O and acetyl acetone iron is 1;

    1;

    0.5;

    Step 4, the settled solution obtained by 100ml step 3 is put into reactor, after sealing, is heated to 150 DEG C, protectsWarm 2h, 200 DEG C are warming up to 2-4 DEG C/min heating rate afterwards, 4h are incubated, afterwards with 3-6 DEG C/min heating rate literTemperature is incubated 3h to 235 DEG C, then 200 DEG C of insulation 2h is cooled to 5-7 DEG C/min cooling rate, finally again with 3-6 DEG C/minHeating rate be warming up to 235 DEG C, be incubated 7h, after the completion of question response, reactor taken out, is allowed to be cooled to room temperature, the dropWarm speed is 3-6 DEG C/min, and the black powder of gained centrifuged into 10min, 8000~10000r/min of rotating speed, and use is anhydrousRespectively washing three times, is dried in vacuo 24h at 50~70 DEG C, obtains the first product for ethanol and deionized water;

    The products of 5g first and 5-10g aniline monomers are added into the solution of DBSA, ultrasonic disperse 65min, shapeInto the second product, the mass ratio of first product and DBSA is 1-1.5;

    8-15;

    3g ammonium persulfates are dissolved in 80-120ml distilled water, are slowly dropped in the second product, stirring reaction 15h, reactionAfter end, filter, it is colourless to filtrate with distilled water, ethanol washed product respectively, 50~70 DEG C of 24~36h of vacuum drying, obtainAbsorbing material;

    Absorber Bandwidth of the absorbing material below reflection loss -10dB is up to 4.8-5.1GHz, and maximum reflection loss reachesTo -24dB.

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