Ni/TiO2-SiO2 Catalyst Synthesis for Terpinen-4-ol
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Solution Overview
Problem
Current methods for synthesizing terpinen-4-ol face challenges due to poor catalytic performance and difficulty in catalyst recovery, particularly with the scarcity of 1,4-cineole resources and high by-product formation in hydrogenation steps.
Innovation Solution
A sol-gel method is employed to create a dual-functional Ni/TiO2—SiO2 catalyst through a series of steps involving hydrolysis, centrifugation, roasting, and reduction, enabling isomerization and hydrogenation reactions with high efficiency and catalyst recyclability.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Reliability
If traditional catalysts are used for hydrogenation, then the reaction can proceed, but the catalytic performance is poor and the catalyst is difficult to recover
Solution Approach 1:
The patent uses a composite catalyst system consisting of Ni nanoparticles supported on TiO2-SiO2 binary oxide. This composite structure combines the hydrogenation activity of Ni with the structural stability and ease of separation properties of the TiO2-SiO2 support, achieving both high catalytic performance and easy recovery through centrifugation.
Solution Approach 2:
The TiO2-SiO2 binary oxide support provides a porous structure that allows for efficient mass transfer while maintaining catalyst stability. The porous nature of the support material enables the Ni nanoparticles to be accessible to reactants while being easily separable from the reaction mixture through centrifugation.
2Productivity
If 1,4-cineole is used as raw material, then the synthesis is simple and efficient, but the resource is scarce
Solution Approach 1:
The patent changes the raw material from scarce 1,4-cineole to abundant terpinolene from turpentine. By adjusting the catalyst system and reaction conditions (temperature, pressure, solvent), the synthesis pathway is optimized to maintain high efficiency while using readily available raw materials.
3Manufacturing precision
If epoxidation or photosensitive oxidation is performed before hydrogenation, then terpinen-4-ol can be obtained, but many by-products are formed
Solution Approach 1:
The patent combines isomerization and hydrogenation into a single catalytic step using the dual-functional Ni/TiO2-SiO2 catalyst. This merging of reaction steps eliminates intermediate isolation and reduces by-product formation that would occur in sequential epoxidation-hydrogenation processes.
Solution Approach 2:
The Ni/TiO2-SiO2 catalyst exhibits multi-functionality, performing both isomerization of terpinolene and subsequent hydrogenation to produce terpinen-4-ol. This dual functionality in a single catalyst system improves selectivity and reduces by-products compared to separate catalytic 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 method achieves a 99% conversion rate and 70% selectivity for terpinen-4-ol production with reduced by-products, ensuring a simple, pollution-free process and high yield.
Implementation Method 1
Tetraethyl silicate is added to the mixed solution of ethanol, water and alkali twice, and hydrolyzed at 20-50° C. 1-6 h to get SiO2 emulsion; Tetrabutyl titanate is added dropwise to the above solution, and hydrolyzed at 50-100° C. for 2-8 h to obtain TiO2—SiO2 binary oxide emulsion
Implementation Method 2
the binary oxide emulsion is centrifuged, washed, dried and roasted; After the hydrogenation reaction is completed, the solution after the reaction is centrifuged to recover the catalyst
Implementation Method 3
The binary oxide emulsion is centrifuged, washed, dried and roasted at 300-700° C. for 2-8 hours to obtain solid TiO2—SiO2 binary oxide; Dry at 70-110° C., roast at 300-700° C. for 2-8 h
Implementation Method 4
The Ni/TiO2—SiO2 catalyst can be obtained by reducing under hydrogen flow
Implementation Method 5
Terpinolene epoxide and Ni/TiO2—SiO2 catalyst is added into the tank reactor, mixed and stirred evenly, the temperature is slowly raised to a certain temperature for isomerization reaction
Implementation Method 6
after the isomerization and cooling to another certain temperature, hydrogen gas is introduced for hydrogenation reaction
Data Source
AI summary
The present invention discloses a nickel/titanium oxide-silicon oxide catalyst for synthesizing terpinene-4-ol as well as a preparation method and method of synthesizing terpinene-4-ol using the same. The preparation method includes the steps of catalyst preparation, terpinene-4-ol synthesis and the like are disclosed in the present invention. The preparation method includes the following steps: firstly, preparing a mixed colloid of TiO2 and SiO2 by using a sol-gel method, and then centrifuging, washing, drying and roasting is performed to prepare a TiO2—SiO2 binary oxide; then, preparing Ni/TiO2-SiO2 by dipping in a nickel nitrate solution, and preparing a supported catalyst by drying and roasting; and finally, adopting a terpinolene-4, 8-epoxide a raw material, carrying out isomerization under the dual catalytic action of TiO2-SiO2 and Ni of the supported catalyst, and carrying out hydrogenation to prepare terpinene-4-ol. The preparation method can combine isomerization and hydrogenation reaction on the same catalyst, has good selectivity on terpinene-4-ol, and is simple to operate and high in product yield.