Method for manufacturing carbon microspheres by using waste macromolecules

A technology of carbon microspheres and polymers, which is applied in the field of making waste polymers into carbon microspheres, can solve the problems of relatively harsh reaction conditions, products containing a large amount of impurities, and difficult to be widely used, and achieve low cost, The effect of uniform product scale and controllable production scale

Inactive Publication Date: 2010-09-01
UNIV OF SCI & TECH OF CHINA
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  • Description
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  • Application Information

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Problems solved by technology

[0004] The application range of the product obtained by this type of reaction is relatively narrow, the recovery rate is not very high, the experimental process is more complicated, and it is difficult to be widely used. The obtained product contains a lot of impurities and cannot be used directly, and the post-processing is troublesome

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  • Method for manufacturing carbon microspheres by using waste macromolecules
  • Method for manufacturing carbon microspheres by using waste macromolecules
  • Method for manufacturing carbon microspheres by using waste macromolecules

Examples

Experimental program
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Embodiment 1

[0019] Example 1. Preparation of carbon spheres in supercritical carbon dioxide

[0020] Weigh 1.50g of polyester (PET) flakes and 12g of dry ice, place them in an autoclave with a capacity of 20ml, and seal; heat to 650°C at a heating rate of 10°C / min, keep warm for 3 hours, cool to room temperature, and turn on the high pressure After the remaining carbon dioxide is released, a black powdery solid product is obtained. The remaining organic matter in the product is washed away with absolute ethanol, filtered, and then the solid powder is dried in an oven at 60°C for 6 hours to obtain the product.

[0021] Product composition can be analyzed by X-ray diffraction OK, the X-ray diffraction analysis results are as follows figure 1 As shown in middle line 1: the peak positions of the two diffraction peaks of the product prepared by PET are at 25.3° and 43.6° respectively, corresponding to the (002) and (100) planes of graphite respectively, and the peak broadening at 25.3° is ob...

Embodiment 2

[0024] Embodiment 2. The impact of reaction conditions (temperature, time, etc.) on the product——taking PET as an example

[0025] Weigh several portions of each 1.50g polyester (PET) sheet and 12.0g dry ice, place each in an autoclave with a capacity of 20ml, seal it; heat it to 500°C, 600°C and 650°C respectively at a heating rate of 10°C / min. ℃, after 3 hours of heat preservation, cool to room temperature, open the autoclave, release the residual carbon dioxide, wash the obtained black powdery solid product with absolute ethanol to remove the remaining organic matter in the product, filter, and then the solid powder Dry in an oven at 60°C for 6 hours.

[0026] Field emission scanning electron microscopy showed that the products prepared above were all spherical, but the surface of the carbon microspheres obtained when the temperature was relatively low (500 ° C) or the reaction time was short (1 hour) was relatively rough. When the temperature rose to 600 The surface of ca...

Embodiment 3

[0028] Example 3. Preparation of layered carbon spheres by high-temperature annealing of carbon microspheres

[0029] Weigh 1 to 3 grams of carbon spheres prepared in Example 1, put them into a corundum crucible, place them in the center of a corundum tube furnace, add heat-insulating refractory bricks at both ends of the tube to keep warm, seal, and evacuate to 1% to 1000% Atmospheric pressure; heat up to 1500°C at a heating rate of 10°C / min, keep warm for 60 minutes, cool to room temperature, ventilate to balance the pressure, and turn on the tube furnace to obtain a light black powdery solid product.

[0030] X-ray diffraction (XRD) analysis shows that the (002) diffraction intensity of graphite in the product is obviously stronger, and the peak width shrinks, indicating that the degree of graphitization is significantly enhanced; The data are in contrast, indicating that the number of sp3 carbon hybridization defects in the product increases with the annealing reaction.

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Abstract

The invention discloses a method for manufacturing carbon microspheres by using waste macromolecules as raw materials. The method is characterized by comprising the following steps of: sealing 75 to 300g/L of waste polyester, polypropylene or polyethylene and 300 to 600g/L of dry ice into a stainless steel autoclave based on the volume of the autoclave, heating the mixture to between 500 and 650 DEG C, preserving the heat for 180 minutes, and then cooling the mixture to room temperature to obtain micro-scale carbon spheres; annealing the prepared micro-scale carbon spheres for 1 hour under the vacuum condition of 1,500 DEG C to further obtain laminated carbon microspheres; and performing oxidation treatment of a Hummers method on the laminated carbon microspheres for 24 to 72 hours to obtain ellipsoidal laminated graphite carbon oxide microspheres. The method can improve the yield of solid carbon and greatly reduce the formation of carbon dioxide, and is suitable for industrialized production; and the obtained product has wide application prospect in the fields of adsorption and desorption, lithium ion batteries, catalyst carriers and the like.

Description

technical field [0001] The invention belongs to the technical field of recycling waste polymers to prepare carbon nanomaterials, in particular to a method for preparing micron-sized carbon spheres, layered carbon microspheres and ellipsoidal layered graphite oxide carbon microspheres by using waste polymer plastics. Background technique [0002] With the development of industry and the progress of society, organic polymer materials are more and more widely used in daily life. Among them, polyester, polypropylene and polyethylene (respectively referred to as PET, PP and PE) gradually constitute an important part of solid waste due to their excellent properties and wide commercial applications (such as beverage bottles, packaging, etc.), which are harmful to the environment. had a serious impact. Therefore, it is particularly important to develop effective recycling methods for organic polymer materials such as PET. [0003] The recovery method of existing waste polyester ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 陈乾旺魏凌志于斌星
Owner UNIV OF SCI & TECH OF CHINA
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