Epoxy Resin Composition Phosphate Neutralization Process
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Solution Overview
Problem
The existing processes for producing aliphatic and cycloaliphatic epoxy resins face challenges such as high content of undesirable partially epoxidized products, reduced mechanical properties, and elevated viscosity due to residual monoglycidyl ether and oligomers, which affect the acid resistance and reactivity of the resin products.
Innovation Solution
A novel process involving azeotropic epoxidation of aliphatic or cycloaliphatic hydroxyl-containing materials with epihalohydrin, using a stoichiometric excess of a base compound and a non-Lewis acid catalyst, followed by neutralization with a phosphate agent to minimize residual alkalinity and separate the epoxy resin composition, thereby reducing the content of monoglycidyl ether and hydrolyzable chlorides.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional epoxidation processes are used to produce aliphatic and cycloaliphatic epoxy resins, then the resin can be manufactured, but the product contains high content of undesirable partially epoxidized products (monoglycidyl ether) and oligomers
Solution Approach 1:
The patent applies preliminary action by adding the phosphate ester neutralizing agent during the epoxidation reaction itself, rather than attempting to remove impurities afterward. The phosphate ester converts residual base and hydrolyzable chlorides to water-soluble salts in situ, enabling direct aqueous extraction of impurities including monoglycidyl ether and oligomers, thereby achieving high purity without complex post-separation processes
Solution Approach 2:
The phosphate ester acts as an intermediary substance that mediates between the epoxidation reaction and the purification process. It neutralizes base and hydrolyzable chlorides to form water-soluble phosphate salts, which serve as intermediates that facilitate the aqueous extraction of impurities, thereby simplifying the overall separation process while achieving high product purity
2Reliability
If fractional vacuum distillation is used to remove monoglycidyl ether from the epoxy resin product, then the acid resistance improves, but excessive diglycidyl ether is also removed leading to elevated viscosity and reduced reactivity
Solution Approach 1:
The patent applies the extraction principle by using aqueous extraction to selectively remove monoglycidyl ether and oligomeric impurities from the epoxy resin product. The phosphate ester treatment creates water-soluble salts that enable selective partitioning of impurities into the aqueous phase while leaving the desired diglycidyl ether product in the organic phase, thereby improving acid resistance without removing excessive product or elevating viscosity
Solution Approach 2:
The patent applies parameter changes by modifying the chemical environment through phosphate ester treatment, which changes the solubility parameters of impurities. The conversion of residual base and hydrolyzable chlorides to water-soluble phosphate salts alters the partitioning behavior of monoglycidyl ether and oligomers, enabling their selective removal into aqueous phase while maintaining the reactivity and viscosity characteristics of the diglycidyl ether product
3Productivity
If known processes are used to produce ACE resin products, then the resin can be manufactured, but catalysts and solvents must be removed before the resin can be used in subsequent operations
Solution Approach 1:
The patent applies continuity of useful action by integrating the neutralization and purification steps into the epoxidation reaction itself. The phosphate ester is added during the reaction, and the aqueous extraction is performed immediately afterward without isolating intermediate products, thereby eliminating separate catalyst removal and solvent recovery steps while maintaining continuous productive flow
Solution Approach 2:
The patent applies merging by combining multiple functions into a single integrated process: the phosphate ester simultaneously neutralizes residual base, converts hydrolyzable chlorides to water-soluble salts, and enables aqueous extraction of impurities. This merges neutralization, purification, and product isolation into one continuous operation, eliminating the need for separate catalyst removal and solvent recovery steps
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 results in an ACE resin composition with low viscosity, improved shelf life, and enhanced curable epoxide content, allowing for the production of thermosets with improved mechanical properties and reduced yellowing and chalking, suitable for industrial-scale production without the need for additional solvents or equipment changes.
Implementation Method 1
neutralizing the resultant reaction mixture containing the ACE resin composition product with a phosphate neutralizing agent sufficient to partially neutralize the basic acting substance
Implementation Method 2
subjecting the reaction mixture of step (III) above to a separation process to recover the ACE resin composition product from the neutralized fluid medium
Data Source
AI summary
A process for preparing an aliphatic or cycloaliphatic epoxy resin composition including the steps of: (I) reacting a mixture of the following components: (a) an aliphatic or cycloaliphatic hydroxyl-containing material, (b) an epihalohydrin, (c) a stoichiometric excess of a base compound or basic acting substance, (d) a catalyst, and (e) optionally, a solvent; wherein the reacting step (I) is carried out under reaction conditions sufficient to form a crude aliphatic or cycloaliphatic epoxy resin composition product in the resultant reaction mixture; (II) neutralizing the resultant reaction mixture of step (I) containing the crude aliphatic or cycloaliphatic epoxy resin composition product with a phosphate neutralizing agent sufficient to partially neutralize the base or basic acting substance and to form a neutralized fluid medium containing aliphatic or cycloaliphatic epoxy resin composition product; (III) removing at least a portion of unreacted epihalohydrin from the reaction mixture of step (II); and (IV) subjecting the reaction mixture of step (III) above to a separation process to recover the aliphatic or cycloaliphatic epoxy resin composition product from the neutralized fluid medium; wherein the aliphatic or cycloaliphatic epoxy resin composition product yield is greater than about 70 percent.