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Method for producing phenolic resin based foam carbon with secondary curing method

A phenolic resin and secondary curing technology, which is used in the preparation of foam carbon, can solve the problems of large sample shrinkage, long preparation time, and difficulty in obtaining complete products, and achieve simple process operation, complete sample structure, and heat insulation. excellent effect

Active Publication Date: 2009-05-13
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the interest and energy of researchers are concentrated on coal-based, asphalt-based, coal tar and petroleum-based, and there is little research on phenolic resin-based foam carbon.
In the 1960s and 1970s, although researchers had made preliminary research on phenolic resin-based foam carbon, there were generally a series of problems such as long preparation time, large shrinkage of samples during carbonization, severe cracking, and difficulty in obtaining complete products. More problems, resulting in products far from meeting the application requirements
At the same time, it is difficult to prepare phenolic resin-based foam carbon samples with large size and regular shape.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: At normal temperature and pressure, first fully dissolve 100g of thermoplastic phenolic resin and 10g of hexamethylenetetramine with 1000mL of absolute ethanol, pour it into an open container, place it on a sample holder, and put it in high temperature in an autoclave. Nitrogen gas was introduced to keep the pressure inside the kettle at 0.8MPa, and the temperature was heated at a rate of 0.2°C / min. When heated to 180°C, start to release the pressure slowly at a rate of 0.5MPa / h, so that the pressure in the kettle is slowly reduced to normal pressure. During the depressurization process, the temperature was kept constant at 180°C. After the depressurization, the temperature was continued to be heated to 250°C at a rate of 0.2°C / min to solidify and form, and the density of 102g was prepared to be 0.13g / cm 3 phenolic-based foam cured body. Then the foam cured body was ground into 150 mesh powder, then added to the ethanol solution containing 10g of 213 thermo...

Embodiment 2

[0021] Embodiment 2: make 102g0.13g / cm with example one 3 phenolic resin-based foam cured body. Then the foam cured body was ground into 200 mesh powder, then added to the ethanol solution containing 10g of 214 thermosetting phenolic resin (the mass percent concentration of the resin was 15%), stirred fully to make a uniform slurry. Dry the slurry in an oven at 60°C, then put it into a mold for pre-compression molding at a pressure of 10 MPa, and heat it to 200°C for curing. Finally, put the cured sample into a carbonization furnace, heat and carbonize it to 1000°C with a temperature rise program of 0.5°C / min in an atmosphere of high-purity nitrogen as a protective gas, and keep the temperature constant for 30 minutes to obtain a density of 0.62g / cm 3 phenolic resin-based carbon foam.

Embodiment 3

[0022] Example 3: At normal temperature and pressure, first fully dissolve 100g of thermoplastic phenolic resin and 8g of hexamethylenetetramine with 500mL of methanol to prepare the prepared raw materials, pour them into an open container, put them on the sample holder, and put them in In high temperature and high pressure autoclave. Nitrogen gas was introduced to keep the pressure inside the kettle at 2.5MPa, and the temperature was heated at a rate of 0.3°C / min. When heated to 200°C, start to release the pressure slowly at a rate of 0.2 MPa / h, so that the pressure in the kettle is slowly reduced to normal pressure. During the depressurization process, the temperature is kept constant at 200°C, and after the pressure relief, continue to heat up to 250°C at a heating rate of 0.3°C / min to solidify and form, and the prepared 103g density is 0.24g / cm 3 phenolic resin-based foam cured body. Then the foam cured body was ground into 150 mesh powder, then added into the methanol s...

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Abstract

The invention relates to a method for preparing phenolic resin base foam carbon by using the secondary solidification method, which comprises the following steps: uniformly dissolving thermoplastic phenolic resin and hexamethylene tetramine by using an organic solvent at the normal temperature, placing in a high-temperature high-pressure autoclave, pressurizing to keep the pressure within the scope of 0.8 to 2.5 MPa, heating to 250 to 300 DEG C according to a certain temperature procedure to be foamed and solidified, and preparing a preparing phenolic resin base foam solidified body; then grinding the foam solidified body into a powder shape, adding phenolic resin to be as a binding agent, heating and molding in a mould; and solidifying and pressing into a regular shape; and finally placing a sample after being pressed into a carbonization furnace to be heated and charred according to a certain temperature procedure and preparing the preparing phenolic resin base foam carbon. The invention has advantages of large dimension and regular appearance.

Description

[0001] Field [0002] The invention belongs to a method for preparing foamed charcoal, in particular to a method for preparing phenolic resin-based foamed charcoal by a secondary curing method. Background technique [0003] Foam carbon is a special new type of porous light carbon material with small and interpenetrating pores, large specific surface area and wide range of density changes. This three-dimensional network structure composed of interconnected cell walls gives it unique properties in terms of acoustics, optics, electricity, heat and dynamics. Foamed carbon has been developed for decades. It was first developed by American Walterford in the late 1960s. This foamed carbon is made by pyrolysis and carbonization of thermosetting resin, which is a carbon skeleton or network glass structure. In the 1990s, a new generation of foamed carbon appeared. Its research direction mainly focused on the preparation of foamed carbon by substituting pitch and coal for other foam sol...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 郭全贵雷世文史景利刘朗宋进仁翟更太
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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