Preparation method of porous carbon material

A technology of porous carbon materials and copolymers, which is applied in the field of preparation of porous carbon materials, can solve problems affecting the performance and stability of porous carbon materials, the formation of complex pore structures, and the influence of porous carbon materials Effects of decomposition temperature and heat treatment time, ease of industrial mass production, reduction of pollution and corrosion of equipment

Active Publication Date: 2014-12-24
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, polyvinylidene chloride is used to prepare porous carbon materials, which generally contains unreacted chlorine atoms, which affects the thermal and chemical stability of porous carbon materials during use. At the same time, due to the low hardness of polyvinylidene chloride, It makes it easy to produce closed cells during the preparation of porous carbon materials, and it is difficult to control the pore size, which affects the performance and stability of porous carbon materials
Moreover, HCl will be produced during the heating dechlorination process of polyvinylidene chloride, and the time required for the dechlorination process is longer, resulting in a long production cycle, and the thermal decomposition temperature is required to be as high as 1000 ° C, resulting in high energy consumption; while using microwave dechlorination method, although the required time is shortened, it is more difficult to mass-produce
In addition, during the preparation of porous carbon materials from polyvinylidene chloride, the HCl produced will inevitably corrode equipment and pollute the environment.
However, purely using polyvinyl chloride to prepare porous carbon materials, due to the insufficient chlorine content in the molecular structure, leads to a low ring formation rate after the removal of chlorine, the strength of porous carbon materials is reduced, and the pore structure is complex and difficult to control, which affects the performance of porous carbon materials. Performance and stability, difficult to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take by weighing chlorinated polyvinyl chloride (Zibo City Linzi Yixiang Chemical Co., Ltd., model: T-500, chlorine content is 60wt.%) powder 42kg, LiOH9kg, methyl methacrylate and styrene copolymer 9kg, at 200rpm rotating speed After mixing at low speed for 10 minutes, extrude and granulate through a twin-screw extruder with a length-to-diameter ratio of 35:1 (manufacturer: Qingdao Kechuang Plastic Machinery Co., Ltd.). The temperature of the chemical section is 200°C, the temperature of the compression section is 210°C, and the temperature of the die is 180°C. The feeding speed of the material is controlled so that the residence time of the material in the twin-screw extruder is 4 minutes to obtain a granulated material. Put the obtained pellets into an oven under inert gas N 2 In the atmosphere, the temperature was raised from 25°C to 600°C at a heating rate of 20°C / min, kept at a constant temperature for 2 hours, then raised to 800°C at a heating rate of 15°C / min, c...

Embodiment 2

[0039] Take by weighing chlorinated polyvinyl chloride (Zibo City Linzi Yixiang Chemical Co., Ltd., model: J-700, chlorine content is 65wt.%) powder 32kg, NaOH4kg, methyl methacrylate and acrylate copolymer 2.5kg, at 300rpm After mixing for 11 minutes at a rotating speed, extrude and granulate through a twin-screw extruder with a length-to-diameter ratio of 35:1 (manufacturer: Qingdao Kechuang Plastic Machinery Co., Ltd.), and set the temperature of the mixing section of the twin-screw extruder at 190°C. The temperature of the plasticizing section is 200°C, the temperature of the compression section is 210°C, and the temperature of the head is 180°C. The feeding speed of the material is controlled so that the residence time of the material in the twin-screw extruder is 5 minutes to obtain a granulated material. Put the obtained granulated material into an oven, in an inert gas Ar atmosphere, start to heat up from 25°C to 650°C at a heating rate of 25°C / min, keep the temperature...

Embodiment 3

[0041] Take by weighing chlorinated polyvinyl chloride (Zibo Linzi Yixiang Chemical Co., Ltd., model: T-500, chlorine content is 62wt.%) powder 38kg, KOH6kg, methyl methacrylate and styrene copolymer 3kg, methacrylic acid Methyl ester and acrylate copolymer 3kg, after mixing at 400rpm rotating speed for 5min, extrude and granulate through twin-screw extruder (manufacturer: Qingdao Kechuang Plastic Machinery Co., Ltd.) with aspect ratio 35:1, set twin-screw The temperature of the mixing section of the extruder is 190°C, the temperature of the plasticizing section is 200°C, the temperature of the compression section is 210°C, and the temperature of the head is 180°C. The residence time was 6 minutes to obtain granules. Put the obtained pellets into an oven under inert gas N 2 In / Ar mixed gas atmosphere, start to heat up from 25°C to 700°C at a heating rate of 30°C / min, keep the temperature constant for 4 hours, then raise the temperature to 900°C at a heating rate of 35°C / min,...

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Abstract

The invention discloses a preparation method of a porous carbon material. The preparation method comprises the following steps: stirring and mixing chlorinated polyvinyl chloride, alkali metal hydroxides and methacrylate copolymers in parts by weight, and extruding at the temperature of 190-210 DEG C to obtain a granulating material; then increasing the temperature of the granulating material from 25 DEG C to 800-900 DEG C in an inert gas atmosphere at two-stage heating rate for carbonization, and then reducing the temperature to 25 DEG C at the cooling rate of 20-40 DEG C/min to obtain a carbonized material; then immersing the carbonized material into an aromatic substance for 2-4 hours, then increasing the temperature from 25 DEG C to 900-1000 DEG C in the inert gas atmosphere at the two-stage heating rate, keeping constant temperature for 3-4 hours, and then reducing the temperature to 25 DEG C at the cooling rate of 15-30 DEG C/min to obtain the porous carbon material. The preparation method disclosed by the invention has the advantages of simple process, environmental protection, easiness for industrialization and stability in product property.

Description

technical field [0001] The invention relates to a method for preparing a porous carbon material, in particular to a method for preparing a porous carbon material by using chlorinated polyvinyl chloride as a main raw material. Background technique [0002] Porous carbon material is a new type of non-polar carbon adsorbent material developed in the 1960s. Porous carbon materials have uniform pore size distribution, high chemical stability and gas selectivity. At present, porous carbon materials have been widely used in environmental protection, chemical industry, petroleum industry, food processing, hydrometallurgy, pharmaceutical refining, military protection, etc. each field. [0003] There are a wide range of raw materials for preparing porous carbon materials, mainly including organic polymers (polyvinylidene chloride resin, phenolic resin, etc.), various coals and coal-based derivatives (lignite, bituminous coal, anthracite, etc.), biomass (wood, shell, bagasse, etc.), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 付铁柱张成德
Owner JUHUA GROUP TECH CENT
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