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Regeneration method of amination catalyst of polyetheramine used for polyether polyol hydro-amination

A technology of alcohol hydrogen amine and polyether multi-component, which is applied in the field of regeneration of amination catalysts for the preparation of polyether amines by hydrogen amination of polyether polyols, and can solve the problem of catalyst activity reduction, destruction of alumina support structure and dissolution Active components, catalyst deactivation and other issues to achieve the effect of improving activity

Active Publication Date: 2018-04-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The common problem of the above-mentioned amination catalyst: the activity of the catalyst decreases with the increase of the use time during use, that is, the catalyst is deactivated
In the washing process of this patent, a large amount of organic solvent is used to wash the catalyst, which has the problems of solvent waste and solvent recovery cost; while the impregnation process uses a concentrated nitric acid solution with an acid concentration of 15-30% to impregnate the catalyst, which destroys the structure of the alumina carrier and dissolves the activity. The problem of components; during the roasting process, air or nitrogen or a mixture of air and nitrogen in any proportion is used for high-temperature roasting, which solves the problem of carrier alumina rehydration and will lead to a decrease in the dispersion of active components and sintering of active components

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Washing step: add the deactivated catalyst into the acetic acid solution with a concentration of 5wt% according to the solid-to-liquid volume ratio of 1:1, heat to reflux for 8 hours, filter, wash until neutral, and dry.

[0050] (2) Roasting step: under normal pressure, place the amination catalyst obtained by washing and drying in a fixed-bed reactor and raise the temperature to 400°C at a heating rate of 3°C / min. A hydrogen peroxide solution with a concentration of 16wt% was used for charcoal regeneration, and the roasting time was 5 hours until no CO2 was detected in the tail gas, and the temperature was lowered to obtain a roasted and regenerated amination catalyst.

[0051] (3) Reduction step: under normal pressure, the fixed bed reactor is heated to 200°C, the heating rate is 0.5°C / min, and the hydrogen / nitrogen gas mixture with a volume ratio of 1:40 is fully reduced for 5 hours, and the temperature is lowered to obtain the reduction Regenerated amination ca...

Embodiment 2

[0055] (1) Washing step: Add the deactivated catalyst into the acetic acid solution with a concentration of 30wt% according to the solid-to-liquid volume ratio of 1:5, heat to reflux for 10 hours, filter, wash until neutral, and dry.

[0056] (2) Roasting step: under normal pressure, place the amination catalyst obtained by washing and drying in a fixed-bed reactor and raise the temperature to 300°C at a heating rate of 1°C / min. A hydrogen peroxide solution with a concentration of 20 wt% is used for charcoal regeneration, and the roasting time is 10 hours, until no CO2 is detected in the tail gas, and the temperature is lowered to obtain a roasted and regenerated amination catalyst.

[0057] (3) Reduction step: under normal pressure, the fixed bed reactor is heated to 100°C, the heating rate is 0.8°C / min, and the hydrogen / nitrogen gas mixture with a volume ratio of 1:10 is fully reduced for 15 hours, and the temperature is lowered to obtain the reduction Regenerated amination ...

Embodiment 3

[0061] (1) Washing step: add the deactivated catalyst into the acetic acid solution with a concentration of 20wt% according to the solid-to-liquid volume ratio of 1:8, heat to reflux for 5 hours, filter, wash until neutral, and dry.

[0062] (2) Roasting step: under normal pressure, place the amination catalyst obtained by washing and drying in a fixed-bed reactor and raise the temperature to 450°C at a heating rate of 5°C / min. A hydrogen peroxide solution with a concentration of 15 wt% is used for charcoal regeneration, and the roasting time is 8 hours, until no CO2 is detected in the tail gas, and the temperature is lowered to obtain a roasted and regenerated amination catalyst.

[0063] (3) Reduction step: under normal pressure, the fixed bed reactor is heated to 250°C, the heating rate is 1°C / min, and the hydrogen / nitrogen gas mixture with a volume ratio of 1:20 is fully reduced for 8 hours, and the temperature is lowered to obtain the reduction Regenerated amination catal...

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Abstract

The invention discloses a regeneration method of an amination catalyst of polyetheramine used for polyether polyol hydro-amination. The method comprises the following steps: A) adding an inactivated amination catalyst in an organic acid solution, heating the material for backflow, filtering the material, washing the material, and drying the material; B) performing carbon burning regeneration on the amination catalyst obtained through washing and drying treatment under existence of hydrogen peroxide to obtain the amination catalyst after roasting regeneration; and C) using hydrogen for reducingthe amination catalyst after roasting regeneration to obtain the amination catalyst after reduction regeneration. The regeneration processing method solves the problem of inactivation of the amination catalyst due to coking even carbon formation, active ingredient copper sintering of the catalyst, and Ni0 crystal-phase aggregation. The regeneration method mainly used for preparing the amination catalyst of polyetheramine for polyether polyol hydro-amination.

Description

technical field [0001] The present invention relates to a method for regeneration of an amination catalyst used for the hydroamination of polyether polyols to prepare polyetheramines, more precisely, it relates to alumina as a carrier, selected from Ni, Co, Cu and Pd Two or more metals are active components selected from Zr, Cr, Mo, Fe, Zn, Sn, Ce, Mg, Mn, La, Hf, Sr, V, Mn, W, Pb, Pt, Ag, Rh, Ru, Bi, Nd, Sb and Be additives in the catalyst composed of more than one metal or its oxides are used in the hydrogenation of polyether polyols to prepare polyether amine amination reaction deactivation after regeneration, The invention belongs to the technical field of catalysts. Background technique [0002] Polyether amine, also known as amino-terminated polyether (ATPE for short), is a kind of polyoxyalkylene compound whose molecular main chain is polyether skeleton and the end is blocked by amino group. Most of these amino-terminated polyethers use polyether (polyethylene glyco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/96B01J38/02B01J38/10B01J38/16B01J38/62C07C213/02C07C217/08C08G65/328C08G65/48
CPCB01J23/8993B01J23/96B01J38/02B01J38/10B01J38/16B01J38/62C07C213/02C08G65/328C08G65/48C07C217/08Y02P20/584
Inventor 任树杰张聪颖李鑫刘振国唐磊吴健姜庆梅曹善健黎源
Owner WANHUA CHEM GRP CO LTD
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