Vacuum Distillation of Organic Solvents and Phenolic Inhibitors

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Solution Overview

Problem

In the semiconductor manufacturing industry, organic solvents like ethers and esters are prone to peroxide formation, leading to contamination, defects, and safety hazards, with existing peroxide inhibitors introducing metallic and high-boiling impurities that worsen the issue.

Innovation Solution

A method involving the co-purification of organic solvents and phenolic peroxide formation inhibitors, where the inhibitor's boiling point is within a specific range relative to the solvent's, using thermal purification processes like distillation under reduced pressure to create a purified mixture that minimizes peroxide formation and impurities.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If industrial peroxide inhibitors are added to organic solvents, then peroxide formation is minimized, but metallic and high-boiling impurities contaminate the solvent

Engineering Contradiction:
Improveperoxide formation preventionVSAvoidmetallic and high-boiling impurities
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The invention changes the physical-chemical parameters of the purification process by conducting distillation at reduced pressure (vacuum conditions). This allows the solvent and phenolic inhibitor to be purified at lower temperatures, preventing decomposition and avoiding the formation of metallic and high-boiling impurities while effectively removing peroxides through the controlled boiling point difference between components

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention extracts and removes harmful peroxide impurities from the organic solvent-inhibitor mixture through vacuum distillation. By exploiting the boiling point difference between peroxides (which boil at lower temperatures) and the desired solvent-inhibitor mixture, peroxides are selectively separated and removed in the distillate, leaving a purified product

Inventive Principle:
Principle #2Taking out (Extraction)

2Object-affected harmful factors

If standard distillation is used to purify organic solvents, then peroxides are removed, but the process requires high temperatures that may cause decomposition

Engineering Contradiction:
Improveperoxide removalVSAvoiddistillation temperature
Core Design Contradiction:
Object-affected harmful factorsVSTemperature

Solution Approach 1:

The invention fundamentally changes the pressure parameter of the distillation process from atmospheric to reduced pressure conditions. This parameter change allows the same purification effect to be achieved at significantly lower temperatures, preventing thermal decomposition of heat-sensitive organic solvents and phenolic inhibitors while maintaining effective peroxide removal through the altered vapor-liquid equilibrium

Inventive Principle:
Principle #35Parameter changes

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 effectively reduces peroxide content and impurities in the solvent mixture, enhancing semiconductor manufacturing by minimizing defects and safety risks while maintaining the purity of electronic devices.

Implementation Method 1

heating the organic solvent and the phenolic peroxide formation inhibitor to a temperature causing the organic solvent and phenolic peroxide formation inhibitor to vaporize

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

condensing the vaporized organic solvent and phenolic peroxide formation inhibitor to provide a purified mixture

Methodology Applied
Scientific EffectCondensation: Condensation

Data Source

PatentUS10370320B2Purification methods
Publication Date: 2019.08.06 DUPONT ELECTRONIC MATERIALS INT LLC
  • US10370320B2 patent drawing

AI summary

Provided are purification methods, comprising: (a) providing an organic solvent and a phenolic peroxide formation inhibitor, wherein the organic solvent has a first boiling point at standard atmospheric pressure (bp1) and the phenolic peroxide formation inhibitor has a second boiling point at standard atmospheric pressure (bp2) that satisfy the following inequality (I):bp2≤(1.10)(bp1)  (I); and(b) heating the organic solvent and the phenolic peroxide formation inhibitor to a temperature causing the organic solvent and phenolic peroxide formation inhibitor to vaporize, and (ii) condensing the vaporized organic solvent and peroxide formation inhibitor to provide a purified mixture of the organic solvent and peroxide formation inhibitor. The methods find particular use in the purification of solvents that are useful in process chemicals for the manufacture of semiconductor devices.