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Catalyst for synthesizing morpholine from diethylene glycol and preparation method thereof

A catalyst and a technology for diethylene glycol are applied in the field of catalysts for synthesizing morpholine from diethylene glycol and the field of preparation thereof, which can solve the problems of low selectivity of morpholine, and achieve high catalytic activity, low preparation cost and good hydrothermal stability. Effect

Active Publication Date: 2021-11-02
ANHUI HAOYUAN CHEM IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problem of unstable performance and low morpholine selectivity of diethylene glycol synthesis morpholine catalysts at present, the invention provides a composite catalyst, which has stable catalytic performance, good catalyst activity and selectivity, and is easy to manufacture

Method used

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  • Catalyst for synthesizing morpholine from diethylene glycol and preparation method thereof
  • Catalyst for synthesizing morpholine from diethylene glycol and preparation method thereof
  • Catalyst for synthesizing morpholine from diethylene glycol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of diethylene glycol synthesis morpholine catalyst:

[0026] (1) Carrier preparation: put weighed 0.1g of boron, 1.0g of SBA-15, 15mL of absolute ethanol and 5.0g of isopropyl titanate into a 50mL beaker and mix well to form a suspension I, and then continue to the suspension Add 5 mL of absolute ethanol and 2 mL of deionized water to liquid I to obtain a mixed solution, then adjust the pH value of the mixed solution to 3 with 10% dilute nitric acid aqueous solution with a pH value of 3, and continue stirring until it forms a stable and transparent gel II. The gel II was aged at room temperature for 24 h, dried at 85 °C for 4 h, and finally calcined at 550 °C for 2 h to obtain white powder TiO 2 / SBA-15;

[0027] Weigh 26g of aluminum nitrate nonahydrate, 50mL of ethanol and 5mL of deionized water to prepare mixed solution III, and white powder TiO 2 / SBA-15 soaked in the above mixed solution III for 8 hours, after filtering, put the filter cake...

Embodiment 2

[0035] The preparation method of diethylene glycol synthesis morpholine catalyst:

[0036] (1) Carrier preparation: put weighed 0.1g of boron, 1.0g of SBA-15, 15mL of absolute ethanol and 5.0g of isopropyl titanate into a 50mL beaker and mix well to form a suspension I, and then continue to the suspension Add 5 mL of absolute ethanol and 2 mL of deionized water to liquid I to obtain a mixed solution, then adjust the pH value of the mixed solution to 3 with 10% dilute nitric acid aqueous solution with a pH value of 3, and continue stirring until it forms a stable and transparent gel II. The gel II was aged at room temperature for 12 h, dried at 85 °C for 4 h, and finally calcined at 550 °C for 2 h to obtain white powder TiO 2 / SBA-15;

[0037] Weigh 26g of aluminum nitrate nonahydrate, 50mL of ethanol and 5mL of deionized water to prepare mixed solution III, and white powder TiO 2 / SBA-15 soaked in the above mixed solution III for 1 hour, dried in an oven at 40°C to remove wa...

Embodiment 3

[0045] The preparation method of diethylene glycol synthesis morpholine catalyst:

[0046] (1) Carrier preparation: put weighed 0.1g of boron, 1.0g of SBA-15, 15mL of absolute ethanol and 5.0g of isopropyl titanate into a 50mL beaker and mix well to form a suspension I, and then continue to the suspension Add 5mL of absolute ethanol and 2mL of deionized water to liquid I to obtain a mixed solution, then adjust the pH value of the mixed solution to 4 with 10% dilute nitric acid aqueous solution with a pH value of 3, and continue stirring until it forms a stable and transparent gel II. The gel II was aged at room temperature for 48 h, dried at 85 °C for 4 h, and finally calcined at 550 °C for 2 h to obtain white powder TiO 2 / SBA-15;

[0047] Weigh 26g of aluminum nitrate nonahydrate, 50mL of ethanol and 5mL of deionized water to prepare mixed solution III, and white powder TiO 2 / SBA-15 soaked in the above mixed solution III for 1 hour, dried in an oven at 40°C to remove wate...

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Abstract

The invention discloses a preparation method of a catalyst for synthesizing morpholine from diethylene glycol, and the preparation method of the catalyst comprises the following steps: (1) preparation of a carrier: titanium isopropoxide is used as a titanium source to load TiO2 in a pore channel of a mesoporous material SBA-15 in a dispersed state, and TiO2 / SBA-15 is prepared; pretreating TiO2 / SBA-15 with a mixed solution of aluminum nitrate as an aluminum source, ethanol and water, loading Al2O3 through a hydrothermal synthesis reaction, and finally preparing the Al2O3 / TiO2 / SBA-15 composite carrier; (2) preparing an impregnation liquid, namely preparing a mixed solution A from soluble salt precursors of active components Cu, Ni and Fe and assistants Mn and Mg; and (3) impregnating the Al2O3 / TiO2 / SBA-15 composite carrier in the mixed solution A, and drying and roasting to obtain the supported metal catalyst. The catalyst prepared by the method has the advantages of stable performance, good morpholine selectivity and environmental friendliness.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst for synthesizing morpholine from diethylene glycol and a preparation method thereof. Background technique [0002] The chemical name of morpholine is 1,4-oxazidine. It is a colorless oily liquid at room temperature, which is weakly alkaline, hygroscopic, and has an ammonia odor and slight toxicity. It can be miscible with water to form an azeotrope, easily soluble in aromatic hydrocarbons, alcohols, ethers, benzene, acetone, sesame oil, etc., and slightly soluble in aliphatic hydrocarbons and mineral oils. Because of its special oxygen nitrogen heterocyclic structure, morpholine It has become an intermediate in the synthesis of many fine chemical products and is widely used in the fields of rubber, medicine, coatings and dyes. At present, the main method of producing morpholine is diethylene glycol catalyzed ammonolysis and cyclization method, that is, diethylene gl...

Claims

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Application Information

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IPC IPC(8): B01J29/03C07D295/023C07D295/027
CPCB01J29/0341C07D295/023C07D295/027B01J2229/186Y02P20/584
Inventor 杨帅成
Owner ANHUI HAOYUAN CHEM IND GRP