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Graphene oxide/polyformaldehyde porous microsphere for reinforced master batch and preparation method of porous microsphere

A technology of reinforcing masterbatch and porous microspheres, which is applied in the field of plastic fillers, can solve the problems of low microsphere pore size, cumbersome preparation process, and difficult dispersion of graphene and other fillers, achieving large microsphere pore size, simple process, and inhibiting the tendency of agglomeration Effect

Inactive Publication Date: 2019-02-01
CHENDU NEW KELI CHEM SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the disadvantages of porous microspheres such as graphene and its derivatives such as graphene and its derivatives, which are widely used at present, which are widely used in polymers such as polyoxymethylene, there are defects such as cumbersome preparation process, low microsphere pore size, and difficult dispersion of fillers such as graphene. A graphene oxide / polyoxymethylene porous microsphere and preparation method for reinforcing the masterbatch, thereby effectively improving the dispersion of graphene, the microsphere has a large pore size, and the preparation process is simple

Method used

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  • Graphene oxide/polyformaldehyde porous microsphere for reinforced master batch and preparation method of porous microsphere

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Experimental program
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Effect test

Embodiment 1

[0032] The preparation process is:

[0033] (1) Disperse graphene oxide in water, add dodecylamine, heat and ultrasonically disperse, then filter and freeze-dry to obtain functionalized graphene oxide; wherein, 7 parts by weight of graphene oxide and 92 parts by weight of water , 1 part by weight of dodecylamine; the heating temperature is 41°C, and the ultrasonic dispersion time is 2h;

[0034] (2) Add polyoxymethylene resin into diphenyl ether, stir until fully dissolved to obtain a polyoxymethylene solution, then add the functionalized graphene oxide prepared in step (1), ultrasonically disperse for 1 hour to obtain a mixed solution, and then introduce In the cooling device, put it into a cold trap for quenching treatment to obtain a gel; wherein, 36 parts by weight of polyoxymethylene resin, 59 parts by weight of diphenyl ether, and 5 parts by weight of functionalized graphene oxide; the temperature of stirring is 30 ° C, The time is 12h; the quenching temperature is 0°C,...

Embodiment 2

[0041] The preparation process is:

[0042] (1) Disperse graphene oxide in water, add dodecylamine, heat and ultrasonically disperse, then filter and freeze-dry to obtain functionalized graphene oxide; wherein, 6 parts by weight of graphene oxide and 93 parts by weight of water 1 part by weight of dodecylamine; the heating temperature is 38°C, and the ultrasonic dispersion time is 3h;

[0043] (2) Add polyoxymethylene resin into diphenyl ether, stir until fully dissolved to obtain a polyoxymethylene solution, then add the functionalized graphene oxide prepared in step (1), ultrasonically disperse for 1 hour to obtain a mixed solution, and then introduce In the cooling device, put it into a cold trap for quenching treatment to obtain a gel; wherein, 30 parts by weight of polyoxymethylene resin, 67 parts by weight of diphenyl ether, and 3 parts by weight of functionalized graphene oxide; the temperature of stirring is 30 ° C, The time is 11h; the quenching temperature is 0°C, a...

Embodiment 3

[0050] The preparation process is:

[0051] (1) Disperse graphene oxide in water, add dodecylamine, heat and ultrasonically disperse, then filter and freeze-dry to obtain functionalized graphene oxide; wherein, 8 parts by weight of graphene oxide and 90 parts by weight of water , 2 parts by weight of dodecylamine; the heating temperature is 43°C, and the ultrasonic dispersion time is 1h;

[0052] (2) Add polyoxymethylene resin into diphenyl ether, stir until fully dissolved to obtain a polyoxymethylene solution, then add the functionalized graphene oxide prepared in step (1), ultrasonically disperse for 1 hour to obtain a mixed solution, and then introduce In the cooling device, put it into a cold trap for quenching treatment to obtain a gel; wherein, 40 parts by weight of polyoxymethylene resin, 52 parts by weight of diphenyl ether, and 8 parts by weight of functionalized graphene oxide; the temperature of stirring is 30 ° C, The time is 13h; the quenching temperature is 0°C...

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Abstract

The invention provides a graphene oxide / polyformaldehyde porous microsphere for reinforced master batch and a preparation method of the porous microsphere. The method comprises the following steps: adding graphene oxide and dodecyl amine into water, carrying out ultrasonic dispersion, and carrying out drying to obtain functionalized graphene oxide; then adding the functionalized graphene oxide into a polyformaldehyde solution to obtain a mixed solution, and carrying out quenching treatment in a cold trap to obtain a gel; and finally, immersing the gel in an ethanol solution, and carrying out treatment in a supercritical reaction kettle of CO2 to obtain the graphene oxide / polyformaldehyde porous microsphere. The polyformaldehyde porous microsphere prepared by thermally induced phase separation according to the method is large in pore size and large in specific surface area. Dispersity of graphene oxide is good, so that when the polyformaldehyde porous microsphere is used as reinforced master batch, the contact area between the graphene oxide and a reinforced matrix is remarkably increased, and then the reinforcing effect of the master batch is improved. Moreover, the preparation method is simple in process and can be popularized and applied in a large scale.

Description

technical field [0001] The invention relates to the field of plastic fillers, in particular to a graphene oxide / polyoxymethylene porous microsphere for reinforcing masterbatch and a preparation method thereof. Background technique [0002] Polyoxymethylene (POM) is a highly crystalline polymer, so it has fast crystallization speed, high crystallinity, high elastic modulus, hardness and rigidity, good resistance to repeated impacts, resistance to organic solvents, oil, and Lubricants etc. It is one of the five major engineering plastics, known abroad as "Dura Steel" and "Super Steel". As mentioned above, POM has good mechanical properties and unique wear-resistant and self-lubricating properties, so it is widely used in automobiles, home appliances, electronics, office supplies, and machinery industries. [0003] Polymer porous microsphere is a polymer spherical particle with a porous structure. Due to its controllable pore structure and its special size effect and interfac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/28C08L59/00C08K9/04C08K3/04C08J3/22
CPCC08J3/223C08J3/226C08J9/286C08J2201/0522C08J2359/00C08K3/042C08K9/04Y02P20/54
Inventor 陈庆
Owner CHENDU NEW KELI CHEM SCI CO LTD
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