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Preparation technology of liquid core-mesoporous solid shell composite microsphere catalyst

A composite microsphere and preparation technology, which is applied in the field of preparation technology of liquid core-mesoporous solid shell composite microsphere catalyst, can solve problems such as emulsion damage and achieve high catalytic performance

Active Publication Date: 2018-11-16
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this system has high catalytic efficiency, the reaction can only be carried out at relatively low temperature, pressure and substrate concentration, because increasing the value of these parameters will lead to the coalescence of droplets and the destruction of emulsion

Method used

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  • Preparation technology of liquid core-mesoporous solid shell composite microsphere catalyst
  • Preparation technology of liquid core-mesoporous solid shell composite microsphere catalyst
  • Preparation technology of liquid core-mesoporous solid shell composite microsphere catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, a preparation process of a liquid core-mesoporous solid shell composite microsphere catalyst, the preparation steps are:

[0025] (1) Add 1.41g n-octane containing 0.02g solid emulsifier hydrophobic nano silica to 1-butyl-3-methylimidazolium tetrafluoroborate (0.80g), water (0.20g), CuI (0.017g) and TX-10 (0.05g) in a mixed solution (1.067g), vigorously stirred by a homogenizer for 2 minutes, an ionic liquid in oil (IL / oil) type Pickering emulsion can be formed.

[0026] (2) Disperse the ionic liquid in oil (IL / oil) Pickering emulsion prepared above into 25ml of n-octane solution containing 0.04g of trimethoxysilane, rotate and mix at 50°C for 12 hours, and remove the upper oil phase After that, wash with n-octane for several times to remove excess cross-linking agent on the surface, and then a liquid core-mesoporous solid shell composite microsphere catalyst can be obtained.

[0027] The prepared liquid core-mesoporous solid shell composite microsphere c...

Embodiment 2

[0029] Embodiment 2, a preparation process of a liquid core-mesoporous solid shell composite microsphere catalyst, the preparation steps are:

[0030] (1) Add 2.810g of n-octane containing 0.025g of solid emulsifier hydrophobic nano-silica to 1-propyl-3-methylimidazolium tetrafluoride boron salt (1.80g), water (0.20g), CuI (0.11g) and PluronicF127 (0.15g) in the mixed solution, the homogenizer was vigorously stirred for 2 minutes, and the ionic liquid in oil (IL / oil) type Pickering emulsion could be formed.

[0031] (2) Disperse the ionic liquid in oil (IL / oil) Pickering emulsion prepared above into 50ml of n-octane solution containing 0.10g of butyl orthosilicate, rotate and mix at 55°C for 15 hours, and remove the upper layer of oil After phase, it is washed several times with n-octane to remove excess cross-linking agent on the surface, and the liquid core-mesoporous solid shell composite microsphere catalyst can be obtained.

[0032] The obtained liquid core-mesoporous so...

Embodiment 3

[0033] Embodiment 3, a preparation process of a liquid core-mesoporous solid shell composite microsphere catalyst, the preparation steps are:

[0034](1) Add 4.22g of n-octane containing 0.04g of solid emulsifier hydrophobic nano-silica to 1-butyl-3-methylimidazolium bromide (1.80g), water (0.20g), CuI (0.096g ) and Triton X-100 (0.30g), and vigorously stirred by a homogenizer for 2 minutes, an ionic liquid in oil (IL / oil) type Pickering emulsion can be generated.

[0035] (2) Disperse the ionic liquid in oil (IL / oil) type Pickering emulsion prepared above into 50ml n-octane solution containing 0.12g tetraethyl orthosilicate, rotate and mix at 25°C for 24 hours, remove the upper layer of oil After phase, it is washed several times with n-octane to remove excess cross-linking agent on the surface, and the liquid core-mesoporous solid shell composite microsphere catalyst can be obtained.

[0036] The obtained liquid core-mesoporous solid shell composite microsphere catalyst is ...

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Abstract

The invention relates to a preparation technology of a catalyst, and concretely relates to a preparation technology of a liquid core-mesoporous solid shell composite microsphere catalyst used for a continuous reaction in a fixed bed. The technology comprises the following steps: (1) adding n-octane and a solid emulsifier to a mixed solution of an ionic liquid, water, CuI and a surfactant, and carrying out vigorous stirring by a homogenizer to form an ionic liquid Pickering-in-oil emulsion; and (2) dispersing the prepared ionic liquid Pickering-in-oil emulsion in n-octane containing a cross-linking agent, rotating and mixing the emulsion and the n-octane containing a cross-linking agent at 25-55 DEG C, standing the obtained solution, removing the upper organic phase, and washing the obtained lower layer with n-octane multiple times to remove the excess cross-linking agent from the surface of the lower layer in order to obtain the liquid core-mesoporous solid shell composite microsphere.The catalyst has a high catalytic performance for the cycloaddition reaction of azide-alkyne, has a micrometer scale and a certain mechanical strength, can be used in the continuous reaction in the fixed bed, and has industrial application values.

Description

technical field [0001] The invention relates to the preparation of a catalyst, in particular to a preparation process of a liquid core-mesoporous solid shell composite microsphere catalyst which can be used for fixed-bed continuous reaction. Background technique [0002] As we all know, homogeneous catalysts have the advantages of high catalytic efficiency, high selectivity, and mild reaction conditions, but their disadvantages are that they are difficult to separate, making continuous reactions difficult; while the biggest advantage of heterogeneous catalysts is that the separation process is simple or even does not need to be separated. Moreover, continuous operation can be carried out, which is beneficial to the industrialization process. However, heterogeneous catalysis is less efficient compared to homogeneous catalysis due to mass transfer issues. Therefore, researchers have long tried to build a bridge between the two, hoping to build an ideal catalyst that has both ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/28B01J35/08
CPCB01J31/0292B01J31/28B01J35/51
Inventor 杨恒权郝雅娟侯屹婷
Owner SHANXI UNIV