Aqueous PVP Polymerization Using Sulfur Components

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Solution Overview

Problem

Existing methods for producing aqueous PVP solutions suffer from high formic acid content, color instability, and the need for toxic or undesirable additives like metals, enzymes, or antioxidants, which are problematic for pharmaceutical and cosmetic applications, especially for transparent hair gels.

Innovation Solution

A process involving the use of sulfur components like sulfur dioxide, sulfurous acid, or their salts to reduce residual monomers, maintaining a pH below 6, and subsequent treatment to produce PVP polymers with low formic acid content and improved color stability during storage.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If polymerization is carried out in organic solvents like isopropanol, then the polymer product has low impurity content, but the process requires costly distillation to remove solvent and replace with water, leading to long reactor occupancy time and low space-time yield

Engineering Contradiction:
Improvepurity of polymer productVSAvoidspace-time yield
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention changes the solvent parameter from organic (isopropanol) to aqueous medium, enabling direct polymerization in water without subsequent distillation steps. This parameter change resolves the contradiction by achieving both acceptable purity and high productivity through aqueous-phase polymerization followed by simple filtration.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention extracts the harmful organic solvent from the process entirely, replacing it with water as the polymerization medium. This eliminates the need for distillation and solvent removal steps, directly improving space-time yield while maintaining product purity through filtration of the aqueous reaction mixture.

Inventive Principle:
Principle #2Taking out (Extraction)

2Productivity

If polymerization is carried out in aqueous solution with hydrogen peroxide as initiator, then the process is simpler and more productive, but high hydrogen peroxide concentrations promote formic acid formation and cause yellow coloration

Engineering Contradiction:
Improvepolymerization efficiencyVSAvoidformic acid content and coloration
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The invention changes the pH parameter of the aqueous solution to alkaline conditions (pH 8-10) using ammonia or other bases. This parameter change suppresses formic acid formation and prevents yellow coloration while maintaining high polymerization efficiency with hydrogen peroxide initiator.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces ammonia or other bases as intermediary substances that mediate between the hydrogen peroxide initiator and the polymerization process. These intermediaries maintain alkaline conditions that prevent formic acid formation and coloration while allowing efficient polymerization to proceed.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Reliability

If existing processes are used to produce aqueous PVP solutions, then polymerization can be carried out, but the products have high formic acid content and discolor during storage, requiring toxic additives like metals, enzymes, or antioxidants

Engineering Contradiction:
Improvecolor stability during storageVSAvoidformic acid content
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The invention maintains alkaline pH conditions (pH 8-10) throughout the polymerization and storage process using ammonia or other bases. This parameter change simultaneously achieves low formic acid content and excellent color stability during storage without requiring any toxic additives.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The alkaline ammonia system serves multiple functions simultaneously: it acts as pH regulator, formic acid suppressor, and color stability agent. This self-service approach eliminates the need for separate additives like metals, enzymes, or antioxidants, providing both low formic acid content and color stability.

Inventive Principle:
Principle #25Self-service

4Reliability

If antioxidants are added to prevent oxidation and color changes in PVP solutions, then color stability improves, but large amounts are required because peroxides from polymerization consume the antioxidants

Engineering Contradiction:
Improvecolor stabilityVSAvoidamount of antioxidant required
Core Design Contradiction:
ReliabilityVSQuantity of substance

Solution Approach 1:

The invention applies preliminary anti-action by maintaining alkaline conditions with ammonia from the beginning, which prevents formic acid formation and coloration before they can occur. This preemptive approach eliminates the need for large amounts of antioxidants that would otherwise be consumed by peroxide formation.

Inventive Principle:
Principle #9Preliminary anti-action

Solution Approach 2:

The invention converts the potentially harmful effect of hydrogen peroxide into a beneficial process by operating in alkaline conditions where peroxide decomposition is controlled and does not lead to formic acid formation or coloration. This allows efficient polymerization without requiring excessive antioxidants.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

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

The process effectively reduces formic acid content and enhances color stability in PVP solutions, making them suitable for cosmetic and pharmaceutical applications without the use of toxic additives, ensuring stable and transparent products.

Implementation Method 1

use of sulfur components like sulfur dioxide, sulfurous acid, or their salts to reduce residual monomers

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 2

Producing N-vinylpyrrolidone polymers by free-radical polymerization

Methodology Applied
Scientific EffectFree-radical polymerization: Photopolymerisation

Implementation Method 3

polymerization in the presence of hydrogen peroxide as initiator

Methodology Applied
Scientific EffectDecomposition: Decomposition (biological)

Implementation Method 4

high hydrogen peroxide quantities promote the formation of formic acid in the aqueous system

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentUS9260546B2Producing aqueous solutions of vinyllactam polymers and powders thereof
Publication Date: 2016.02.16 BASF SE

AI summary

Described is a process for producing aqueous solutions of vinyllactam polymers and solids obtainable therefrom by drying, especially polyvinylpyrrolidone, said process comprising using one or more sulfur components selected from the group consisting of sulfur dioxide, sulfurous acid and one or more salts of sulfurous acid, to reduce residual monomer. Also described are vinyllactam polymers obtainable by the process which have good stability in storage, the use of these vinyllactam polymers, and articles of manufacture and preparations comprising these vinyllactam polymers or obtained by use thereof.