Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid alkali

A technology of inorganic oxides and hollow mesopores, applied in the preparation of organic compounds, preparation of oxides/hydroxides, preparation/treatment of rare earth metal compounds, etc., to achieve simple preparation process, easy recycling, and increase mass transfer rate Effect

Pending Publication Date: 2021-02-05
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method of O-alkylation of phenolic compounds has the following disadvantages: ①Stoichiometric strong base is required, such as Na 2 CO 3 、K 2 CO 3 , KOH or NaOH to generate phenol anions, most of these inorganic bases cannot be miscible with organic raw materials, so toxic water-soluble solvents and phase transfer systems have to be used in the selection of reaction solvents, which cause separation problems
However, due to its inert reaction, it needs to be effectively carried out under the catalysis of high temperature and highly active solid base. The solid base reported in the literature can only realize the selective O-alkylation of phenolic compounds under the condition of more than 300 °C. The highest selectivity of O-alkylated products is only 84%, and C-alkylated by-products are inevitably generated

Method used

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  • Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid alkali
  • Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid alkali
  • Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid alkali

Examples

Experimental program
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Embodiment 1

[0041] Example 1 Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid base

[0042] (1) Preparation method of hollow mesoporous inorganic oxide nanosphere solid base

[0043] This embodiment includes the following steps:

[0044] S1. Using 1240 g glucose as the carbon source, prepare a 0.5 M glucose solution with deionized water, place the high-pressure hydrothermal reactor in an electric constant temperature drying oven preheated to 200 °C in advance, and then add the glucose solution to the high-pressure water After reacting for 4 hours in a hot reactor, cool it down to room temperature naturally, filter the dark brown product with suction, and wash the filter cake alternately with deionized water and ethanol until the drop at the lower end of the funnel is colorless, then put it in a constant temperature drying oven and dry it at 65 °C for 12 hours , to obtain 55g nano colloidal carbon spheres;

[0045] Such as figure 1 and figure 2 ...

Embodiment 2

[0056] Example 2 Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid base

[0057] (1) Preparation method of hollow mesoporous inorganic oxide nanosphere solid base

[0058] This embodiment includes the following steps:

[0059] S1. Using 1462g of glucose as the carbon source, prepare a 0.8 M glucose solution with deionized water, place the high-pressure hydrothermal reactor in an electric constant temperature drying oven preheated to 160 °C in advance, and then add the glucose solution to the high-pressure hydrothermal After reacting in the reactor for 2 h, cool down to room temperature naturally, filter the dark brown product with suction, and wash the filter cake alternately with deionized water and ethanol until the drop at the lower end of the funnel is colorless, then put it in a constant temperature drying oven at 60 °C for 12 h, Obtain 100g nano colloidal carbon spheres;

[0060] S2. Dissolve magnesium acetate and zinc acetate in ...

Embodiment 3

[0068] Example 3 Preparation method and application of hollow mesoporous inorganic oxide nanosphere solid base

[0069] (1) Preparation method of hollow mesoporous inorganic oxide nanosphere solid base

[0070] This embodiment includes the following steps:

[0071] S1. Using 78g of sucrose as the carbon source, prepare a 1.5 M sucrose solution with deionized water, place the high-pressure hydrothermal reaction kettle in an electric heating constant temperature drying oven preheated to 175 ℃ in advance, and then add the sucrose solution to the high-pressure hydrothermal After reacting in the reactor for 8 hours, it was naturally cooled to room temperature, and the dark brown product was suction-filtered, and the filter cake was washed alternately with deionized water and ethanol until the drop at the lower end of the funnel was colorless, and then dried in a constant temperature drying oven at 70 °C for 12 hours to obtain 20g nano colloidal carbon spheres;

[0072] S2. Magnes...

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Abstract

The invention belongs to the field of heterogeneous catalysis, and discloses a preparation method of hollow mesoporous inorganic oxide nanosphere solid alkali, which comprises the following steps: adding nano colloidal carbon spheres into an inorganic metal salt solution/inorganic metal salt mixed solution, stirring, adsorbing, filtering, and washing to obtain a hollow mesoporous inorganic oxide carbon sphere precursor; drying the hollow mesoporous inorganic oxide carbon sphere precursor, grinding the dried hollow mesoporous inorganic oxide carbon sphere precursor into powder, and carrying outgradient heating calcination on the powder to obtain hollow mesoporous inorganic oxide nanosphere solid alkali. The invention also discloses an application of the hollow mesoporous inorganic oxide nanosphere solid base prepared by the preparation method. The hollow mesoporous inorganic oxide nanosphere solid base is used for catalyzing selective O-alkylation reaction of phenolic compounds. The hollow mesoporous inorganic oxide nanosphere solid alkali prepared by the method is uniform in particle size, proper in pore diameter and rich in porous structure, can be easily separated from a productafter catalyzing the selective O-alkylation reaction of phenolic compounds, and is convenient to recycle.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis, and in particular relates to a preparation method and application of a hollow mesoporous inorganic oxide nanosphere solid base. Background technique [0002] O-alkylation products of phenolic compounds are widely used in pharmaceuticals, fine chemicals and petrochemicals. Among them, anisole can be used to prepare spices, pesticides, cosmetics and dyes, etc.; diphenol monoethers, such as 2-methoxyphenol, can be used to produce various fine chemicals and valuable synthetic intermediates; 3-methoxy Phenylphenol and 4-methoxyphenol can be used as UV inhibitors, oil antioxidants and polymerization inhibitors. Therefore, the selective synthesis of O-alkylated products of phenolic compounds is particularly important. [0003] The traditional method of O-alkylation of phenolic compounds has the following disadvantages: ①Stoichiometric strong base is required, such as Na 2 CO 3 、K 2 CO 3 , KO...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/18C01G9/00C01F5/06C01F11/04C01G37/02C01F17/229C01F17/10C01G25/02C01G53/00C01G45/12C01B32/15B82Y40/00B01J23/06B01J23/02B01J23/26B01J23/10B01J23/755B01J23/34B01J21/10B01J21/06B01J35/08B01J35/10B01J37/08C07C41/16C07C43/20C07C43/23C07C43/225C07C43/275C07C43/295C07C201/12C07C205/37
CPCC01B13/18C01G9/00C01F5/06C01F11/04C01G37/02C01F17/229C01F17/10C01G25/02C01B32/15C01G53/00C01G45/1207B82Y40/00B01J23/06B01J23/002B01J23/02B01J23/26B01J23/10B01J23/755B01J23/34B01J21/10B01J21/066B01J35/023B01J35/08B01J35/1014B01J35/1061B01J37/088C07C41/16C07C201/12C01P2004/32C01P2004/03C01P2002/85C01P2004/62C01P2006/12C01P2006/16C07C43/20C07C43/23C07C43/225C07C43/275C07C43/295C07C205/37
Inventor 马学兵王旭日
Owner SOUTHWEST UNIVERSITY
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