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Graphite oxide with multiple carbonyl functional groups and preparation method therefor

A polycarbonyl-functional and carbonyl-functional technology, which is applied in the field of graphite oxide with polycarbonyl functional groups and its preparation, can solve the problems of weak stability of hydroxyl and epoxy groups, low ratio of carbonyl and carboxyl, and low stability, and achieves easy modification. and functionalization, the preparation process is simple and easy, and the effect of ensuring the effect of use

Active Publication Date: 2020-02-14
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the large-scale preparation of graphene oxide materials is generally realized by the Hummers method, but the graphite oxide obtained by this method has a low ratio of carbonyl to carboxyl, high content of hydroxyl and epoxy groups and low stability (the stability of hydroxyl and epoxy groups is weak ), making it unable to meet the performance requirements of the catalyst framework or loaded drug delivery, and unable to realize the application in the field of biomedicine
And the application of raw material sodium nitrate in this method will inevitably lead to the generation of toxic gas nitric oxide and nitrogen dioxide, endanger the personal safety of operators, and cannot meet the requirements of the country for green environmental protection

Method used

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  • Graphite oxide with multiple carbonyl functional groups and preparation method therefor
  • Graphite oxide with multiple carbonyl functional groups and preparation method therefor

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Experimental program
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Effect test

Embodiment 1

[0028] The preparation process of the graphite oxide of the present embodiment polycarbonyl functional group is:

[0029] In a 1000mL beaker, add 180mL of 99% low-concentration fuming sulfuric acid, cool down to below 2°C, add 5g of graphite powder, stir for 1h to obtain sulfuric acid intercalated graphite, then cool down to below 2°C, slowly add potassium permanganate 20g, keep at 15±2℃, react for 48h, fully oxidize graphite.

[0030] After the reaction is over, lower the temperature to below 5°C, slowly add 180g of deionized water dropwise, control the temperature below 20°C, stir fully, keep the reaction at 5-20°C for 2 hours, control the temperature at 5-15°C and add 30% hydrogen peroxide (mass percent concentration) 20mL to obtain a soil-gray suspension, which was heated to 30°C for 1 h.

[0031] The suspension is washed with 5% (mass percent concentration) dilute hydrochloric acid by static layering, and then the graphite oxide is washed with deionized water by centrifu...

Embodiment 2

[0034] The preparation process of the graphite oxide of the present embodiment polycarbonyl functional group is:

[0035] In a 50L jacketed glass reactor, add 2400mL of 100% low-concentration fuming sulfuric acid, cool down to below 2°C, add 60g of graphite powder, stir for 2h to obtain sulfuric acid intercalated graphite, then cool down to below 2°C, and slowly add Potassium permanganate 300g, keep at 20±2℃, react for 96h, fully oxidize graphite.

[0036] After the reaction is over, lower the temperature to below 5°C, slowly add 2400g of deionized water dropwise, control the temperature below 20°C, stir well, and when the dropwise addition is complete, keep it at 5-20°C for 3 hours, control the temperature at 5-15°C and add 300mL of 30% hydrogen peroxide, A muddy gray suspension was obtained, and the temperature was raised to 30° C. for 2 h.

[0037] The suspension is washed with 5% dilute hydrochloric acid by static layering, then the graphite oxide is washed with deionized...

Embodiment 3

[0039] The preparation process of the graphite oxide of the present embodiment polycarbonyl functional group is:

[0040] In a 1000mL beaker, add 180mL of 99.9% low-concentration fuming sulfuric acid, cool down to below 2°C, add 6g of graphite powder, stir for 1.5h to obtain sulfuric acid intercalated graphite, then cool down to below 2°C, slowly add permanganate Potassium 24g, keep 20~23℃, react for 58h, fully oxidize graphite.

[0041]After the reaction is over, lower the temperature to below 5°C, slowly add 180g of deionized water dropwise, control the temperature below 20°C, stir well, and after the dropwise addition is completed, keep it at 5-20°C for 4 hours, control the temperature at 5-15°C and add 19.2mL of 30% hydrogen peroxide , to obtain a muddy gray suspension, which was heated to 35° C. for 0.5 h.

[0042] The suspension is washed with 5% dilute hydrochloric acid by static layering, then the graphite oxide is washed with deionized water by centrifugal separation...

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Abstract

The invention relates to graphite oxide with multiple carbonyl functional groups and a preparation method therefor. According to the graphite oxide and the preparation method therefor, the operation is simple, safe and environmentally friendly, novel impurity elements cannot be introduced into the obtained graphite oxide, the use effect of the graphite oxide is ensured; and compared with the Hummers method, reactants are free of sodium nitrate, so that the generation of toxic gases, i.e., nitrogen monoxide and nitrogen dioxide is avoided. Low-concentration fuming sulfuric acid is employed in areaction system, thus, moisture generated from a reaction can be effectively absorbed, the reaction system can be free of moisture, hydroxide radicals and hydrogen ions, and thus, oxidant potassium permanganate functional groups introduced to a basal plane of graphite cannot be substituted with the hydroxide radicals; and the volume and mass of the potassium permanganate functional groups are farlarger than those of the hydroxide radicals, steric hindrance generated by adjacent potassium permanganate functional groups on the basal plane of the graphite is improved, the stability of carbon-to-carbon bonds is lowered, the breakaway of the carbon-to-carbon bonds is caused, carbon atoms are further oxidated to form two carbonyl groups, and thus, the content of the carbonyl groups in the final product graphite oxide is remarkably improved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a graphite oxide with multiple carbonyl functional groups and a preparation method thereof. Background technique [0002] Graphene oxide not only has the single-layer honeycomb hexagonal planar structure of graphene, but also contains a large number of functional groups, such as hydroxyl, carboxyl, epoxy, carbonyl, etc., so it has good dispersibility, hydrophilicity, and surface modification. , Compatibility with polymers and other excellent properties. [0003] At present, the large-scale preparation of graphene oxide materials is generally realized by the Hummers method, but the graphite oxide obtained by this method has a low ratio of carbonyl to carboxyl, high content of hydroxyl and epoxy groups and low stability (the stability of hydroxyl and epoxy groups is weak ), making it unable to meet the performance requirements of the catalyst framework or loaded drug ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/23
CPCC01P2002/85C01B32/23
Inventor 张强杨玉莹秦禄昌范慧清李爽爽
Owner SHANDONG UNIV OF TECH
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