Crude Ester Catalyst Residue Agglomeration Filtration
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Solution Overview
Problem
Existing processes for working up crude esters containing metal-containing esterification catalyst residues face challenges such as long filtration times, reduced yield, and filter cake retention due to the slimy consistency of catalyst residues, which complicates the separation and leads to process inefficiencies and equipment blockages.
Innovation Solution
A process involving the addition of 1 to 10% water to the crude ester to form a suspo-emulsion, followed by conversion to a water-undersaturated state to facilitate the formation of stable agglomerates that can be easily filtered, utilizing emulsification and agglomeration steps to separate the catalyst residues.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Reliability
If filtration is performed on crude ester containing catalyst residues in slimy gel-like form, then catalyst residues can be removed, but filtration time becomes excessively long and ester yield is reduced due to large product retention in filter cake
Solution Approach 1:
The patent changes the physical state of catalyst residues from slimy gel-like form to free-flowing granular form by controlling water content and temperature parameters. By maintaining water content below the solubility limit and operating at temperatures above 100°C, the catalyst residues transform into easily filterable granules, resolving the contradiction between effective removal and fast filtration.
Solution Approach 2:
The patent utilizes phase transition of water from liquid to vapor by operating at temperatures above 100°C under pressure. This prevents water from forming a continuous phase that would cause slimy consistency, instead allowing catalyst residues to form discrete granular particles that filter rapidly while maintaining high yield.
2Reliability
If water is added to crude ester to neutralize acid, then neutralization occurs, but water evaporates immediately causing solid NaOH to precipitate and react more slowly
Solution Approach 1:
The patent performs preliminary action by adding water under pressure at temperatures above 100°C before neutralization begins. This pre-conditioning ensures water remains in liquid phase during base addition, allowing rapid dissolution and reaction. The pressure maintenance prevents premature evaporation, enabling fast neutralization kinetics.
3Reliability
If aqueous base is added at high temperature to neutralize crude ester, then neutralization is effective, but water evaporates causing solid hydroxide precipitation and deposits on pipes and containers
Solution Approach 1:
The patent applies preliminary action by establishing pressure conditions above water vapor pressure before and during base addition. This pre-prevents water evaporation and subsequent hydroxide precipitation, eliminating deposit formation on equipment while maintaining effective neutralization at elevated temperatures.
4Reliability
If large excess of base is used to compensate for slow reaction, then complete neutralization is achieved, but process efficiency is reduced
Solution Approach 1:
The patent changes temperature and pressure parameters to maintain water in liquid phase during neutralization. This enables rapid reaction kinetics with stoichiometric or near-stoichiometric base amounts, achieving complete neutralization without requiring large excesses, thus improving process efficiency and reducing base consumption.
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 rapid and efficient agglomeration of catalyst residues into easily filterable particles, reducing process time and preventing filter clogging, thereby improving throughput and product purity with a low acid number.
Implementation Method 1
the crude ester is mixed with 1 to 10 wt% water in an emulsifying vessel and the water is emulsified in the crude ester to form a suspo emulsion
Implementation Method 2
the water content in the mixture of the suspo emulsion and the pre-filled crude ester is below the solubility limit of water in the crude ester, causing the suspended particulate esterification catalyst hydrolysis products to form stable agglomerates
Implementation Method 3
the agglomerates formed are filtered off
Data Source
Figure 1A~1B
Figure 2
AI summary
In a process for workup of a crude ester comprising esterification catalyst hydrolysis product in suspended particulate form, a) the crude ester is admixed in an emulsifying tank with 1% to 10% by weight of water and the water is emulsified in the crude ester to obtain a suspoemulsion, b) the suspoemulsion from the emulsifying tank is transferred to an agglomerating tank containing an initial charge of water-undersaturated crude ester, such that a water content below the solubility limit of water in the crude ester is established in the mixture of the suspoemulsion and the initial charge of crude ester, as a result of which the suspended particulate esterification catalyst hydrolysis products form stable agglomerates, and c) the agglomerates formed are filtered off.