Ni-Al2O3@Al2O3-SiO2 Coated Catalyst for Butane-1,4-Diol Purification

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Solution Overview

Problem

The separation of cyclic acetal, 2-(4′-hydroxybutoxy)-tetrahydrofuran, from butane-1,4-diol is challenging due to its azeotrope formation with butane-1,4-diol, leading to impurities and quality issues in the hydrogenation process, and existing catalysts lack ideal hydrogenation efficiency and complex preparation processes.

Innovation Solution

A Ni—Al2O3@Al2O3—SiO2 catalyst with a coated structure is developed, where Ni particles are dispersed on an Al2O3 carrier with an Al2O3—SiO2 coating layer, facilitating high selectivity and ease of preparation, and the Al2O3—SiO2 layer is deposited between NiO particles to prevent aggregation and enhance hydrogenation activity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a general-purpose hydrogenation catalyst is used, then the hydrogenation process can proceed, but the hydrogenation effect is not ideal and cyclic acetal cannot be effectively removed

Engineering Contradiction:
Improvehydrogenation efficiencyVSAvoidcatalyst performance
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent modifies the catalyst's chemical composition parameters by incorporating specific ratios of Ni (1-10 wt%), Al2O3 (80-98 wt%), and SiO2 (0.1-5 wt%), and controls particle size parameters (Ni particle diameter 5-20 μm) to optimize both hydrogenation efficiency and cyclic acetal removal capability

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite catalyst material combining Ni metal particles with Al2O3 carrier and SiO2 coating layer, where each component contributes specific functions: Ni provides hydrogenation activity, Al2O3 provides structural support and acidity for hydrolysis, and SiO2 enhances stability and prevents sintering

Inventive Principle:
Principle #40Composite materials

2Reliability

If a Ni—SiO2/Al2O3 catalyst is used to achieve effective hydrolyzation and hydrogenation conversion, then the cyclic acetal can be converted, but the preparation process becomes complicated

Engineering Contradiction:
Improveconversion efficiencyVSAvoidpreparation process complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent merges the hydrolysis function (provided by Al2O3 acidity) and hydrogenation function (provided by Ni) into a single integrated catalyst particle structure, eliminating the need for separate catalysts or multi-step processes while achieving both conversions in one reactor

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent creates local functional zones within the catalyst particle: Ni particles distributed on the Al2O3 surface provide localized hydrogenation sites, while the SiO2 coating layer provides localized stabilization and prevents bulk sintering, achieving high conversion with simple preparation

Inventive Principle:
Principle #3Local quality

3Productivity

If cyclic acetal, 2-(4′-hydroxybutoxy)-tetrahydrofuran remains in the butane-1,4-diol product, then the hydrogenation process can continue, but the purity and chromaticity of the product are seriously affected

Engineering Contradiction:
Improveproduction continuityVSAvoidproduct purity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent converts the harmful cyclic acetal byproduct into a beneficial intermediate that is further transformed into additional butane-1,4-diol product through hydrolysis and hydrogenation reactions catalyzed by the same catalyst, turning a quality problem into a productivity advantage

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The catalyst performs multiple functions simultaneously: it catalyzes the hydrogenation of 1,4-butynediol to butane-1,4-diol, hydrolyzes cyclic acetal to 4-hydroxybutyraldehyde, and hydrogenates the hydrolyzed product back to butane-1,4-diol, achieving both high productivity and high purity in one process

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 catalyst achieves efficient conversion of cyclic acetal to butane-1,4-diol with improved product quality and reduced chromaticity, while maintaining high hydrogenation activity and hydrothermal stability, effectively addressing the separation and purification challenges.

Implementation Method 1

Ni particles are distributed on a surface of an Al2O3 carrier in an amorphous or highly dispersed state as an active component for the catalyst

Methodology Applied
Scientific EffectCatalysis: Catalysis

Implementation Method 2

The catalyst achieves efficient conversion of cyclic acetal to butane-1,4-diol with improved product quality

Methodology Applied
Scientific EffectHydrogenation: Hydrogenation

Implementation Method 3

loading the Al2O3—SiO2 layer in a depositing manner onto a surface of a Ni/Al2O3 catalyst obtained in the impregnation step

Methodology Applied
Scientific EffectDeposition: Deposition (physical)

Implementation Method 4

loading the active component Ni onto the Al2O3 carrier using an impregnation method, Ni being distributed in tetrahedral and octahedral holes on an Al2O3 surface and growing into microcrystalline particles by using the tetrahedral and octahedral holes as nuclei

Methodology Applied
Scientific EffectImpregnation: Adsorption

Implementation Method 5

growing into microcrystalline particles by using the tetrahedral and octahedral holes as nuclei

Methodology Applied
Scientific EffectNucleation: Nucleation

Data Source

PatentUS11504698B2Ni—Al<sub>2</sub>O<sub>3</sub>@Al<sub>2</sub>O<sub>3</sub>—SiO<sub>2 </sub>catalyst with coated structure, preparation method therefor and application thereof
Publication Date: 2022.11.22 SHANXI UNIV
  • US11504698B2 patent drawing
  • US11504698B2 patent drawing

AI summary

A Ni—Al2O3@Al2O3—SiO2 catalyst with coated structure is provided. The catalyst has a specific surface area of 98 m2/g to 245 m2/g, and a pore volume of 0.25 cm3/g to 1.1 cm3/g. A mass ratio of an Al2O3 carrier to active component Ni in the catalyst is Al2O3:Ni=100:4˜26, a mass ratio of the Al2O3 carrier to an Al2O3—SiO2 coating layer is Al2O3:Al2O3—SiO2=100:0.1˜3, and a molar ratio of Al to Si in the Al2O3—SiO2 coating layer is 0.01 to 1. Ni particles are distributed on a surface of the Al2O3 carrier in an amorphous or highly dispersed state and have a grain size less than or equal to 8 nm, and the coating layer is filled among the Ni particles.