Crystallization of n-hexyl UV Filter for Pourable Handling

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Solution Overview

Problem

The existing methods for producing n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate result in a product that crystallizes slowly, requiring heating to convert the melt into a usable form, which is inefficient and inconvenient for handling.

Innovation Solution

A method involving heating the n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate above its melting point, then cooling and stirring it below the melting point to induce crystallization, allowing for the production of pourable or flowable crystalline particles with controlled particle size and high purity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If the product is bottled as melt and crystal growth occurs after storage for about six weeks at room temperature, then the product can be stored and transported, but the user has to heat the entire pack to a temperature above the melting point to remove liquid product, which is inefficient and inconvenient

Engineering Contradiction:
Improveease of handlingVSAvoidcrystallization time
Core Design Contradiction:
Ease of operationVSLoss of time

Solution Approach 1:

The patent applies preliminary action by inducing crystallization during the production process rather than allowing spontaneous crystallization during storage. The melt is cooled and stirred to promote crystal formation before bottling, so that the product is already in a manageable crystalline or semi-crystalline state when packaged, eliminating the need for users to heat the entire pack later.

Inventive Principle:
Principle #10Preliminary action

2Ease of manufacture

If the product is produced as a dry powder embedded in modified starch as protective colloid, then the powder can be redispersed in water, but the protective colloid has to be tolerated in subsequent applications, which may not be desirable

Engineering Contradiction:
Improveease of processingVSAvoidcontamination
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

The patent applies the taking out principle by removing the protective colloid (modified starch) from the final product formulation. Instead of embedding the UV filter in starch, the patent produces the crystalline UV filter directly in its pure form through controlled crystallization, thereby eliminating the need for protective colloids that would contaminate or interfere with subsequent cosmetic applications.

Inventive Principle:
Principle #2Taking out (Extraction)

3Productivity

If the product crystallizes slowly requiring heating to convert the melt into a usable form, then the product can be obtained, but the process is inefficient and inconvenient for handling

Engineering Contradiction:
Improveproduction efficiencyVSAvoidhandling convenience
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The patent applies parameter changes by controlling the temperature and stirring conditions during the crystallization process. The melt is cooled to a specific temperature range and stirred at controlled rates to promote rapid and uniform crystal formation, transforming the slow spontaneous crystallization into a fast, controlled process that produces handleable crystalline product without requiring subsequent heating.

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 enables the rapid and reproducible production of high-purity, crystalline n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate, facilitating its safe and efficient handling and incorporation into cosmetic preparations as a UV filter or free-radical scavenger.

Implementation Method 1

crystallizing out n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate at a temperature below 57°C, wherein the clear melt from process step a) is stirred at a temperature below 57°C until opacity arises

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS9550727B2Method for the crystallization of 2-(4-N,N-diethyl amino-2-hydroxy-benzoyl)-benzoic acid-n-hexyl ester
Publication Date: 2017.01.24 BASF SE
  • US9550727B2 patent drawing

AI summary

The present invention relates to a method for the crystallization of n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate, to a method for the production of pourable or flowable particles of crystalline n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)-benzoate and to specific pourable or flowable particles of crystalline n-hexyl 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoate.