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Preparation method and application method of polyether amine catalyst

A catalyst and polyetheramine technology, which is applied in the field of preparation of catalysts for the synthesis of polyetheramines, can solve the problems of catalyst selectivity and stability to be improved in anti-hydration ability of catalysts, so as to avoid rehydration deactivation, improve selectivity and Excellent stability and use effect

Active Publication Date: 2020-04-07
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technicians in this study found that the catalyst carrier prepared by the above method has certain excellent performance, but the anti-hydration ability of the catalyst, the selectivity and stability of the catalyst still need to be improved

Method used

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  • Preparation method and application method of polyether amine catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: Preparation of CAT-01

[0028] (1) Add 50 parts (mass unit, the same below) of montmorillonite to 350 parts of 5% KNO 3 Put the solution in a four-necked flask, heat it in a water bath at 60°C, and stir at a constant speed for 30 minutes; then filter and wash with deionized water three times, and then put it in a vacuum oven at 110°C for 4 hours to obtain potassium-based montmorillonite.

[0029] (2) Load metal salts containing 5% nickel, 10% cobalt, 10% copper, 8% ruthenium, 5% molybdenum, and 5% lanthanum on 1000 parts of γ-Al by equal volume impregnation method 2 o 3 Above, after impregnation, dry at 80-100°C for 3 hours, and then bake in a muffle furnace at 200-450°C for 8 hours to complete one impregnation.

[0030] (3) Load half the mass of metal salt solution and 500 parts of dimethylamine solution containing 15 parts of potassium-based montmorillonite for one impregnation onto the carrier after one roasting by equal volume impregnation method. Af...

Embodiment 2

[0032] Embodiment 2: Preparation of CAT-02

[0033] (1) Add 50 parts of montmorillonite to 250 parts of 7% KNO 3 Put the solution in a four-neck flask, heat it in a water bath at 60°C, and stir at a constant speed for 30 minutes; then filter and wash with deionized water three times, and then put it in a vacuum oven at 120°C for 2 hours to obtain potassium-based montmorillonite.

[0034] (2) The metal salt containing 10% nickel, 10% cobalt, 10% ruthenium, 3% molybdenum, and 2% lanthanum was loaded onto 1000 parts of γ-Al by equal volume impregnation method 2 o 3 Above, after impregnation, dry at 60-80°C for 4 hours, and then bake in a muffle furnace at 200-450°C for 10 hours to complete one impregnation.

[0035] (3) Load half the mass of metal salt solution used for one impregnation and 500 parts of diethanolamine solution containing 25 parts of potassium-based montmorillonite on the carrier after one roasting by equal volume impregnation method. After impregnation, 60- Dr...

Embodiment 3

[0037] Embodiment 3: Preparation of CAT-03

[0038] (1) Add 50 parts of montmorillonite to 200 parts of 8% KNO 3 Put the solution in a four-necked flask, heat it in a water bath at 60°C, and stir at a constant speed for 30 minutes; then filter and wash with deionized water three times, and then put it in a vacuum oven at 100°C for 4 hours to obtain potassium-based montmorillonite.

[0039] (2) Load metal salts containing 15% nickel, 5% cobalt, 5% copper, 5% ruthenium, 2% molybdenum, and 5% lanthanum on 1000 parts of γ-Al by equal volume impregnation method 2 o 3 Above, after impregnation, dry at 100-120°C for 2 hours, and then bake in a muffle furnace at 200-450°C for 6 hours to complete one impregnation.

[0040] (3) Load half the mass of metal salt solution used for one impregnation and 500 parts of ethylenediamine solution containing 35 parts of potassium-based montmorillonite on the carrier after one roasting by equal volume impregnation method. After impregnation, 100 Dr...

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Abstract

The invention relates to the field of polyether amine preparation, in particular to a preparation method and an application method of a catalyst for synthesizing polyether amine. The preparation method of the polyether amine catalyst comprises the following steps: (1) potassium-based montmorillonite is prepared; (2) primary impregnation is carried out, namely, a supported catalyst comprises an active component and an auxiliary agent, a gamma-Al2O3 carrier is loaded with a metal salt solution containing an active component and an auxiliary agent by adopting an isopyknic impregnation method, anddrying and roasting are carried out to obtain a carrier loaded with the metal oxide; (3) secondary impregnation is carried out, namely, an equal amount of an organic amine solution of the potassium-based montmorillonite obtained in the step (1) is added into a metal salt solution for impregnation which is half of the metal salt solution in the step (2), the carrier loaded with the metal oxide obtained in the step (2) is impregnated, and drying and roasting are carried out to obtain a catalyst; and (4) reduction is carried out, namely, the modified carrier loaded with the metal oxide obtainedin the step (3) is put into a rotary furnace, and H2 is introduced for reduction to obtain the polyether amine catalyst.

Description

technical field [0001] The invention relates to the field of polyetheramine preparation, in particular to a preparation and application method of a catalyst for synthesizing polyetheramine. Background technique [0002] Polyether amine, also known as amino-terminated polyether, is a kind of polyolefin compound with soft polyether backbone and terminated by primary or secondary amino groups. In the 1950s, US2888439 DuPont first reported the synthesis of polyetheramine, and since then, the synthesis methods of polyetheramine have emerged in an endless stream. So far, the synthesis methods of polyetheramine mainly include ammonolysis method, leaving group method, hydrolysis method and aminophenoxy method. At present, the industrial production mainly adopts the ammonolysis method, which is completed by the gaseous mixture of alcohol, ammonia and hydrogen at about 200°C and a certain pressure through the catalysis of copper and nickel. The whole reaction process includes the st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/325C08G65/48
CPCC08G65/3255C08G65/48
Inventor 向松柏王伟松余江陈天园边鑫彦
Owner ZHEJIANG HUANGMA TECH
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