Methacrylic Acid Purification via Controlled Crystallization

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Solution Overview

Problem

Existing methods for purifying methacrylic acid, such as crystallization, struggle to effectively remove aldehydes as impurities, leading to coloration issues and inefficient purification, with unclear optimal operating conditions and challenges in removing secondary components like methanol from the crystal group.

Innovation Solution

A method involving mixing raw methacrylic acid with methanol at a concentration of 3.0 to 3.75% by mass, precipitating crystals in a cooling crystallization vessel, and using a scraper-equipped crystallization apparatus to enhance crystal precipitation and purity, while controlling temperature and solvent concentration for efficient solid-liquid separation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If extraction method or distillation method is used, then most impurities are separated, but aldehydes cannot be sufficiently removed leading to coloration

Engineering Contradiction:
Improvepurity of methacrylic acidVSAvoidcoloration due to aldehyde impurities
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The patent employs crystallization, a phase transition process, to separate methacrylic acid from aldehyde impurities. By controlling the phase change from liquid to solid crystal form, the method achieves selective purification that removes aldehydes effectively, preventing coloration while obtaining high-purity methacrylic acid.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent optimizes specific parameters including methanol concentration (1-35% by mass), temperature conditions, and crystallization time to enhance the removal of aldehyde impurities. By adjusting these parameters, the crystallization process achieves superior purification compared to conventional extraction or distillation methods.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If crystallization method is used with wide concentration range of second component, then aldehydes can be removed, but operating conditions for efficient purification are not clearly defined

Engineering Contradiction:
Improvepurification efficiencyVSAvoidunclear operating conditions
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent systematically investigates and optimizes key parameters including methanol concentration (1-35% by mass), temperature, and crystallization time. By establishing clear parameter ranges and their effects on purification efficiency, the patent provides well-defined operating conditions that resolve the ambiguity in conventional crystallization methods.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs monitoring and optimization based on purification results to refine operating conditions. By measuring purification efficiency and adjusting parameters accordingly, the method establishes clear, optimized operating conditions for efficient aldehyde removal while maintaining reproducibility.

Inventive Principle:
Principle #23Feedback

3Manufacturing precision

If second component is added to crude methacrylic acid, then crystallization can occur, but second component must be finally removed from crystal group

Engineering Contradiction:
Improvecrystal purityVSAvoidsecond component content in crystals
Core Design Contradiction:
Manufacturing precisionVSLoss of substance

Solution Approach 1:

The patent utilizes controlled crystallization phase transition to selectively incorporate methacrylic acid into the crystal structure while excluding the second component (methanol). By optimizing crystallization conditions, the method achieves effective separation where the desired product crystallizes in high purity form, minimizing co-crystallization of the solvent.

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent creates different local environments within the crystallization system - the crystal lattice structure provides a selective environment that accommodates methacrylic acid molecules while excluding methanol molecules. This local structural selectivity enables high-purity crystal formation with minimal second component incorporation.

Inventive Principle:
Principle #3Local quality

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 approach increases the purity of the crystal group after solid-liquid separation and achieves high productivity by optimizing crystal precipitation rates and maintaining high crystal group purity, as demonstrated by specific examples and graphical relationships.

Implementation Method 1

precipitating a crystal of methacrylic acid from a mixed solution containing the raw material methacrylic acid and methanol

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

the crystal of methacrylic acid is precipitated from the mixed solution in a cooling crystallization vessel

Methodology Applied
Scientific EffectCooling: Cooling

Data Source

PatentUS10442747B2Method for purifying methacrylic acid and method for producing methacrylic acid
Publication Date: 2019.10.15 MITSUBISHI CHEM CORP
  • US10442747B2 patent drawing

AI summary

A method for purifying methacrylic acid, including mixing raw material methacrylic acid and methanol; precipitating a crystal of methacrylic acid from the mixed solution; and separating the crystal and mother liquor, wherein the raw material methacrylic acid and methanol are mixed so that a concentration of methanol in the mixed liquid is 3.0 to 3.75% by mass, and the crystal of methacrylic acid is precipitated from the mixed solution in a cooling crystallization vessel.