A kind of graphite oxide with multiple carbonyl functional groups and preparation method thereof

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, inability to meet environmental protection, and endanger the personal safety of operators. The process is simple and easy, easy to modify and functionalize, and the effect of reasonable raw material preparation

Active Publication Date: 2021-09-28
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of graphite oxide with multiple carbonyl functional groups and preparation method thereof
  • A kind of graphite oxide with multiple carbonyl functional groups and preparation method thereof

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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 a graphite oxide with multiple carbonyl functional groups and a preparation method thereof. The operation is simple, safe and environmentally friendly. The obtained graphite oxide will not introduce new impurity elements, ensuring the use effect of graphite oxide. Compared with the Hummers method, there is no sodium nitrate in the reactant, and the generation of toxic gases nitric oxide and nitrogen dioxide is avoided. . The use of low-concentration fuming sulfuric acid in the reaction system can effectively absorb the moisture produced by the reaction, ensuring that there is no moisture, no hydroxide and hydrogen ions in the reaction system, so it can ensure that the oxidant potassium permanganate functional group introduced on the graphite base surface does not It will be replaced by hydroxide. Since the volume and mass of the potassium permanganate functional group are much larger than the hydroxide, the steric hindrance generated by the adjacent potassium permanganate functional group on the graphite base surface becomes larger, reducing the stability of the carbon-carbon bond. The carbon-carbon bond is broken, and the carbon atom is further oxidized to form two carbonyl groups, and the carbonyl content in the final product graphite oxide is significantly increased.

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 Patents(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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