Solvent-Free Ammoximation via Membrane Distribution
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Solution Overview
Problem
Traditional oxime production methods are time-consuming, environmentally harmful, and energy-intensive due to the use of solvents, with low conversion rates and high energy consumption, necessitating a solvent-free and environmentally friendly process.
Innovation Solution
A solvent-free ammoximation process using titanium silicalite (TS-1) catalyst and membrane distribution for ketone ammoximation reactions, where hydrogen peroxide and ammonia are fed through a membrane distributor, optimizing reaction conditions such as temperature, stirring speed, and membrane type to enhance mass transfer and efficiency.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Reliability
If traditional hydroxylamine method is used for oxime production, then the process can be implemented with existing technology, but the process becomes time-consuming and complicated with strong acid corrosion requirements
Solution Approach 1:
The patent changes the chemical parameters of the reaction system by using TS-1 catalyst with hydrogen peroxide instead of traditional hydroxylamine sulfate and strong acids. This parameter change transforms the reaction mechanism, enabling a one-step ammoximation process that reduces production time while maintaining reliability through optimized catalytic conditions
Solution Approach 2:
The patent extracts and eliminates the time-consuming steps from the traditional multi-step hydroxylamine method. By removing the need for separate hydroxylamine preparation and strong acid treatment steps, the process is simplified to a direct one-step reaction, significantly reducing production time
2Productivity
If solvent is added in the ammoximation reaction, then the reaction can proceed efficiently, but the energy consumption increases due to solvent recycling
Solution Approach 1:
The patent extracts and removes the solvent component from the reaction system entirely. By conducting the ammoximation reaction in a solvent-free environment using TS-1 catalyst, the process eliminates the need for solvent addition and subsequent recycling operations, thereby reducing energy consumption while maintaining reaction efficiency
Solution Approach 2:
The patent creates a localized reactive environment at the catalyst surface where the reaction occurs efficiently without bulk solvent. The TS-1 catalyst provides a specific local environment that facilitates the reaction between ketone and hydrogen peroxide, eliminating the need for bulk solvent while maintaining high reaction efficiency
3Ease of manufacture
If solvent is used in the ammoximation reaction, then the reaction can be carried out, but the environmental pollution is aggravated
Solution Approach 1:
The patent extracts and eliminates the harmful solvent component from the process. By implementing a solvent-free ammoximation reaction using TS-1 catalyst, the process removes the source of environmental pollution associated with solvent use and disposal, while maintaining ease of manufacture through a simplified one-step process
Solution Approach 2:
The patent converts the potential harm of solvent use into benefit by eliminating it entirely. The solvent-free condition, which initially might seem to hinder reaction feasibility, actually benefits the environment by eliminating pollution while the TS-1 catalyst ensures the reaction proceeds efficiently
4Ease of manufacture
If water is used as solvent in cyclohexanone ammoximation, then the reaction can proceed, but the conversion rate of cyclohexanone is as low as about 40.0%
Solution Approach 1:
The patent changes the physical state parameter by removing water solvent entirely and conducting the reaction in a solvent-free system. This parameter change, combined with TS-1 catalyst, dramatically improves cyclohexanone conversion rate from 40.0% to above 98.0%, while maintaining process simplicity through direct one-step reaction
Solution Approach 2:
The patent uses TS-1, a composite material combining titanium and silicalite, as catalyst. This composite structure provides unique catalytic properties that enable high conversion rates in solvent-free conditions, overcoming the limitations of water as a solvent while maintaining ease of manufacture
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 process achieves high conversion rates (98% or above) and selectivity for oxime production with minimal environmental impact and energy consumption, producing water as the primary by-product, while eliminating the need for solvent recycling.
Implementation Method 1
a solvent-free green ammoximation process based on membrane distribution
Implementation Method 2
the key point of solvent-free ammoximation reaction is to realize the effective mass transfer for solution-to-solution and solution-to-catalyst
Implementation Method 3
The one-step synthesis of oxime product can be realized with ketone ammoximation reaction catalyzed by the TS-1 in the presence of hydrogen peroxide
Data Source
AI summary
The invention relates to a solvent-free green ammoximation process based on membrane distribution with a procedure as: adding TS-1 catalyst and ketone into a reactor in advance; setting the stirring speed and reaction temperature; after reaching the set temperature, adding a certain amount of ammonia and hydrogen peroxide into a reaction solution, wherein the hydrogen peroxide is fed in a way of using membrane as a distributor, the ammonia is fed in a continuous or semi-continuous manner; oxime is produced upon the reaction. The advantages of the invention include the mild reaction conditions, high reacting efficiency, simple operation and environmentally-friendly process. And there is no need to add any solvent during the reaction process. During the ammoximation reaction, both the conversion rate of the ketone and the selectivity of the oxime can be over 98.0%.