Polyacrylonitrile Macroporous Carbon Monolith Preparation

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Solution Overview

Problem

Current methods for preparing polyacrylonitrile-based three-dimensional macroporous carbon monoliths face challenges such as complex processing routes, high costs, poor environmental protection, and uncontrollable pore structures, particularly due to the high viscosity and close softening and decomposition temperatures of polyacrylonitrile, limiting their large-scale production and application.

Innovation Solution

A method involving dissolving polyacrylonitrile in an organic solvent, evaporating part of the solvent to form sheets, hot-pressing these sheets into blocks, and then using supercritical carbon dioxide for physical foaming, pre-oxidation, and carbonization under controlled conditions to produce a polyacrylonitrile-based three-dimensional macroporous carbon monolith, with hot-pressing at 140-160°C and solvent content within 35-55 wt% to ensure uniformity and prevent decomposition.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If hard templating method is used to prepare polyacrylonitrile-based three-dimensional macroporous carbon monoliths, then pore structure controllability is improved, but processing complexity and cost increase significantly

Engineering Contradiction:
Improvepore structure controllabilityVSAvoidprocessing complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention extracts and removes the complex templating step entirely, adopting a template-free approach where pore structures are formed directly during carbonization through controlled decomposition of polyacrylonitrile, eliminating the need for separate template preparation, impregnation, and removal steps

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention performs preliminary action by pre-oxidizing the polyacrylonitrile before carbonization to create a more stable structure that facilitates uniform pore formation during subsequent carbonization, ensuring better pore structure controllability without requiring complex templating

Inventive Principle:
Principle #10Preliminary action

2Ease of manufacture

If polyacrylonitrile is heated above its decomposition temperature to enable hot-pressing, then molding capability is improved, but material decomposition occurs

Engineering Contradiction:
Improvemolding capabilityVSAvoidmaterial integrity
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The invention changes the temperature parameter from above decomposition temperature to below decomposition temperature (140-160°C), and compensates by adjusting pressure parameters and adding solvent control to achieve molding capability without material decomposition

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces organic solvent as an intermediary that plasticizes polyacrylonitrile, reducing its viscosity and enabling hot-pressing at lower temperatures below the decomposition point, thus achieving molding capability while maintaining material integrity

Inventive Principle:
Principle #24Intermediary (Mediator)

3Ease of operation

If polyacrylonitrile is dissolved in organic solvent with high solvent content to improve processability, then viscosity decreases and processing becomes easier, but product uniformity deteriorates

Engineering Contradiction:
ImproveprocessabilityVSAvoidproduct uniformity
Core Design Contradiction:
Ease of operationVSManufacturing precision

Solution Approach 1:

The invention optimizes the solvent content parameter to a specific range (35-55 wt%) that balances processability and product uniformity, and controls evaporation rate and hot-pressing parameters to ensure uniform solvent removal and prevent defects

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention implements feedback control by monitoring solvent content during evaporation and adjusting processing parameters accordingly to maintain optimal conditions for both processability and product uniformity

Inventive Principle:
Principle #23Feedback

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method results in a polyacrylonitrile-based three-dimensional macroporous carbon monolith with uniform pore structure, adjustable pore density and size, low density, and good conductivity, facilitating large-scale production and environmental friendliness, while maintaining the mechanical strength and porosity of the final product.

Implementation Method 1

dissolving polyacrylonitrile in an organic solvent

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

evaporating part of the solvent out to obtain sheets

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 3

hot-pressing these sheets into blocks

Methodology Applied
Scientific EffectThermal compression: Compression

Implementation Method 4

using supercritical carbon dioxide for physical foaming

Methodology Applied
Scientific EffectSupercritical fluid formation: Supercritical Fluid

Implementation Method 5

supercritical carbon dioxide for physical foaming

Methodology Applied
Scientific EffectDiffusion: Diffusion

Implementation Method 6

pre-oxidation

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 7

carbonization

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Data Source

PatentUS11845665B2Preparation method of polyacrylonitrile-based three-dimensional macroporous carbon monolith
Publication Date: 2023.12.19 SHANDONG UNIV
  • US11845665B2 patent drawing
  • US11845665B2 patent drawing
  • US11845665B2 patent drawing

AI summary

A preparation method of a polyacrylonitrile-based three-dimensional macroporous carbon monolith. The process route of the method includes the following steps: completely dissolving polyacrylonitrile in an organic solvent, then carrying out drying, cutting, hot-pressing and punching to obtain a foam precursor, next, preparing a polyacrylonitrile foam with a controllable pore structure by a supercritical carbon dioxide batch foaming method, and finally carrying out pre-oxidation and carbonization treatment to obtain the polyacrylonitrile-based three-dimensional macroporous carbon monolith. The preparation method of the polyacrylonitrile-based three-dimensional macroporous carbon monolith of the present invention is simple, easy to control, environmentally friendly and low in cost, thus, the present invention is conducive to large-scale production of the carbon monolith. The prepared polyacrylonitrile-based three-dimensional macroporous carbon monolith has the characteristics of uniform and controllable pore structure and good conductivity, and has a broad application prospect. The method has simple steps, convenient operation and high practicability.