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Preparation method of cassava-starch-based grading-pore carbon microsphere material

A technology of cassava starch and hierarchical pore carbon, which is applied in the direction of carbon preparation/purification to achieve the effect of low price and simple process

Inactive Publication Date: 2014-03-19
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is basically no research on the hierarchical pore structure of carbon materials.

Method used

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  • Preparation method of cassava-starch-based grading-pore carbon microsphere material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Enzymatic hydrolysis of tapioca starch to prepare porous starch: Weigh 30 grams of tapioca starch, add it to a sandwich bottle filled with 45 ml of buffer solution (HAc-NaAc) with a pH of 4.7, preheat it in a water bath at 42 degrees for 10 minutes, and then Add 0.60 g of glucose and 0.15 g of amylase into the system, keep stirring in a 42-degree water bath for 24 hours for enzymolysis reaction, wash with deionized water to neutral after reaction, and freeze-dry to obtain porous starch.

[0026] Then the porous tapioca starch is pretreated: take 25 grams of porous starch and put it into a 180 degree oven for pretreatment for 4 hours.

[0027] Then the porous tapioca starch after pretreatment is put into tube furnace, under nitrogen atmosphere, gas flow rate is 30 milliliters / minute, rises to 500 degrees from room temperature by 2 degrees / minute heating rate and is incubated 1 hour;

[0028] Mechanically mix the carbonized porous tapioca starch with potassium hydroxid...

Embodiment 2

[0032] According to the enzymatic hydrolysis method described in Example 1, porous starch was obtained as a raw material for pretreatment: 25 grams of porous starch was weighed, and pretreated in an oven at 200 degrees for 4 hours.

[0033] Put the pretreated porous tapioca starch into a tube furnace, under a nitrogen atmosphere, the gas flow rate is 70 ml / min, and the temperature rises from room temperature to 600 degrees at a rate of 2 degrees per minute and is kept for 1 hour.

[0034] Mechanically mix the carbonized porous tapioca starch with potassium hydroxide, wherein the carbon-to-alkaline ratio (mass ratio) is 1:8, put it into a tube furnace, and in a nitrogen atmosphere, the gas flow rate is 100 ml / min, press 5 Degrees per minute The heating rate is raised from room temperature to 950 degrees and kept for 3 hours. After the product is cooled, it is washed with dilute hydrochloric acid, then washed with distilled water until the pH value of the washing solution is 6, a...

Embodiment 3

[0036] According to the enzymatic hydrolysis method described in Example 1, porous starch was obtained as a raw material for pretreatment: 25 grams of porous starch was weighed, and pretreated in an oven at 200 degrees for 16 hours.

[0037] Put the pretreated porous tapioca starch into a tube furnace, under a nitrogen atmosphere, the gas flow rate is 30 ml / min, and the temperature rise rate is 1 degree / min from room temperature to 700 degrees and kept for 1 hour.

[0038] Mechanically mix the carbonized porous tapioca starch with potassium hydroxide, wherein the carbon-to-alkaline ratio (mass ratio) is 1:5, put it into a tube furnace, and in a nitrogen atmosphere, the gas flow rate is 100 ml / min, press 4 Degrees per minute The heating rate is raised from room temperature to 950 degrees and kept for 3 hours. After the product is cooled, it is washed with dilute hydrochloric acid, then washed with distilled water until the pH value of the washing solution is 7, and then dried at...

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Abstract

The invention relates to a method for preparing a carbon microsphere material with a grading-pore structure by utilizing cassava starch as a raw material. The preparation method comprises the following steps of (I) placing the cassava starch into a water bath at the temperature of 42DEG C to carry out enzymatic hydrolysis with glucolase and amylase with the mass ratio of 1: 1 to 5: 1 for 24 hours, washing the mixture by utilizing deionized water to be neutral, and carrying out freeze drying on the mixture to obtain the porous starch; (II) weighing the porous starch with a given quantity, placing the weighed porous starch into a drying box at the temperature of 180 to 250 DEG C to be pretreated for 4 to 24 hours; placing the pretreated porous starch into a tubular furnace, heating the porous starch at a temperature increasing speed of 1 to 2 DEG C / min to 500 to 700 DEG C under the nitrogen flow rate of 30 to 70 ml / min, and preserving the heat for 1 hour; mechanically and uniformly mixing the carbonized porous starch with the potassium hydroxide according to the carbon-alkali ratio of 1: 2 to 1: 8, placing the mixture into the tubular furnace, heating the mixture at the temperature increasing speed of 2 to 5 DEG C / min to 850 to 950 DEG C under the condition that the nitrogen flow rate is 60 to 100ml / min, and preserving the heat for 1 hour to 3 hours, washing the obtained product after being cooled by utilizing diluted hydrochloric acid and distilled water until the pH value is 6 to 7, and drying at the temperature of 120 DEG C to obtain the grading-pore carbon microsphere.

Description

technical field [0001] The invention relates to a method for preparing a carbon microsphere material with a hierarchical pore structure by using cassava starch as a raw material, and belongs to the field of inorganic material preparation. Background technique [0002] Spherical carbon materials, as an important new type of functional-based carbon materials, have won the favor and attention of researchers for their regular spherical structure, ultra-high bulk density, high specific surface area, and good electrical and thermal conductivity. The technical field has a broad application space and development value. [0003] During the research on the formation of coke in the 1960s, it was found that pitch compounds would undergo mesophase transformation during heat treatment to form mesophase carbon microspheres. Mesophase carbon microspheres have many excellent properties, such as: self-sintering performance, chemical inertness, high bulk density, excellent electrical and ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 金顶峰杨潇彭晓领金红晓王新庆李静洪波葛洪良
Owner CHINA JILIANG UNIV
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