Phosphinimide Titanium Catalyst Synthesis via Room Temperature Route
Find Innovative SolutionsGenerate Solutions
Solution Overview
Problem
Existing methods for synthesizing titanium complexes like R13P═N—TiCl3 and (1-R2-Indenyl)Ti(N═PR13)Cl2 are difficult to scale up to commercially significant levels due to the need for low temperature steps and time-consuming filtration processes, limiting their yield and efficiency.
Innovation Solution
A new synthetic route involving the combination of TiCl3(OR) with R13P═N—SiMe3 to form R13P═N—TiCl3, followed by reaction with a 1-substituted indene and lithium di-isopropylamide to produce (1-R2-Indenyl)Ti(N═PR13)Cl2, eliminating the need for low temperature steps and filtration, and allowing for high-yield production at large scales.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If previous methods for synthesizing titanium complexes are used, then the catalysts can be made with correct composition, but the synthesis is difficult to scale up due to low temperature steps and filtration requirements
Solution Approach 1:
The invention changes the reaction parameters by using TiCl3(OR) instead of traditional titanium sources and conducting the reaction at room temperature without low temperature steps. This parameter change eliminates the need for specialized temperature control equipment and simplifies the overall process while maintaining catalyst composition accuracy
Solution Approach 2:
The invention extracts and eliminates the filtration step from the synthesis process by using a reaction system that produces soluble products and byproducts, allowing direct use of the reaction mixture without solid-liquid separation. This removes a major source of process complexity and enables easier scaling
2Productivity
If previous synthesis methods are used, then catalyst composition can be controlled, but processing time is increased due to filtration steps
Solution Approach 1:
The invention removes the filtration step entirely from the synthesis pathway by designing a reaction system where all products remain in solution. This extraction of the time-consuming filtration operation directly increases synthesis speed and reduces processing time while maintaining catalyst quality
Solution Approach 2:
The invention enables continuous processing by eliminating discrete separation steps like filtration. The reaction mixture can be directly used in subsequent catalytic processes or stored without interruption, maintaining continuous useful action and reducing overall processing time
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 facile production of active phosphinimide ligated olefin polymerization catalysts at commercially relevant scales, improving yield and reducing processing time and complexity.
Implementation Method 1
combining TiCl3(OR) with an approximately equimolar amount of R13P═N—SiMe3 in the presence of solvent, to give as reaction products the R13P═N—TiCl3 and RO—SiMe3
Implementation Method 2
combining a 1-substituted indene 1-R2—C9H7 with an approximately equimolar amount of lithium di-isopropylamide to give a 1-substituted indenide 1-R2—C9H6 anion
Implementation Method 3
combining the 1-substituted indenide 1-R2—C9H6 anion with the R13P═N—TiCl3 to give (1-R2-Indenyl)Ti(N═PR13)Cl2
Data Source
AI summary
Methods to make R13P═N—TiCl3 and (1-R2-Indenyl)Ti(N═PR13)Cl2, where R1 is independently selected from C1-30 hydrocarbyl radical which is unsubstituted or further substituted by one or more halogen atom, a C1-8 alkoxy radical, a C6-10 aryl radical, a C6-10 aryloxy radical, an amido radical, a silyl radical, and a germanyl radical; P is phosphorus; N is nitrogen (and bonds to the metal M); R2 is a substituted or unsubstituted alkyl group, a substituted or an unsubstituted aryl group, or a substituted or unsubstituted benzyl group, wherein substituents for the alkyl, aryl or benzyl group are selected from alkyl, aryl, alkoxy, aryloxy, alkylaryl, arylalkyl and halide substituents. The method to make R13P═N—TiCl3 combines a titanium species TiCl3(OR) where R is an alkyl or aromatic group, with a trimethylsilyl phosphinimide compound R13P═N—SiMe3 in the presence of solvent, to give the titanium complex R13P═N—TiCl3. The method to make (1-R2-Indenyl)Ti(N═PR13)Cl2 consists of deprotonating 1-R2-indene with an appropriate base, followed by reaction with R13P═N—TiCl3.