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Method for preparing polyether amine by hydroamination of polyether polyol

A technology of polyether polyols and alcohol hydroamines, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc. It can solve the problems of poor catalyst stability, poor catalyst activity, and inability to realize continuous production.

Active Publication Date: 2021-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] From the above review, it can be seen that the use of catalysts in the prior art for the amination of polyether polyols to produce polyetheramines has one or more problems such as poor catalyst activity, poor catalyst stability, inability to realize continuous production, low conversion rate, and low yield of primary amines. multiple aspects of the problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] The catalyst is 10%Co-2%Re / Al 2 o 3 . Weigh 8.8 grams of 20-40 mesh Al 2 o 3 , dried at 120°C for 4 hours before use, and 20ml of the configuration contains 4.94 grams of Co(NO 3 ) 2 ·6H 2 O, 0.29 g NH 4 ReO 4 , an aqueous solution of 1.92 g of β-cyclodextrin, with which the above-mentioned Al 2 o 3 The carrier was air-dried naturally, dried at 100°C for 4h, calcined at 600°C for 4h, and the heating rate was 4°C / min.

[0081] Weigh 4g of the above-mentioned catalyst (20-40 mesh) and place it in the middle of the fixed-bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MPa, temperature 450°C, hydrogen volume space velocity 500h -1 , Time 2h. The reaction conditions are: pressure 6MPa, temperature 170°C, hydrogen volume space velocity 100h -1 , PPG230 (polyoxypropylene ether, average molecular weight about 230g / mol): NH 3 =1:10 (molar ratio), PPG230 liquid hourly space velocity 0.6h -1 . Af...

Embodiment 2

[0084] The catalyst is 10%Ni-10%Co-1%Re-1%Ru-0.5%Ce / Al 2 o 3 . Weigh 7.8 grams of 20-40 mesh Al 2 o 3 , dried at 120°C for 4 hours before use, and 20ml of configuration containing 4.95 grams of Ni(NO 3 ) 2 ·6H 2 O, 4.94 g Co(NO 3 ) 2 ·6H 2 O, 0.14 g NH 4 ReO 4 , 0.26 g RuCl 3 ·3H 2 O, 0.15 g Ce(NO 3 ) 3 ·6H 2 O, an aqueous solution of 4.08 g of ethylenediamine, impregnating the above-mentioned Al with this aqueous solution 2 o 3 The carrier was air-dried naturally, dried at 100°C for 4h, calcined at 400°C for 6h, and the heating rate was 5°C / min.

[0085] Weigh 4g of the above-mentioned catalyst (20-40 mesh) and place it in the middle of the fixed-bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MPa, temperature 400°C, hydrogen volume space velocity 500h -1 , time 2h. The reaction conditions are: pressure 8MPa, temperature 200°C, hydrogen volume space velocity 200h -1 , PPG230 (polyoxypro...

Embodiment 3

[0088] The catalyst is 20%Ni-2%Re / SiO 2 . Weigh 7.8 grams of 100 mesh SiO 2 , dried at 120°C for 4 hours before use, the SiO 2 Disperse in water to form a suspension, and stir at a medium speed at a constant temperature of 50°C. Configuration 20ml contains 9.91 grams of Ni (NO 3 ) 2 ·6H 2 O, 0.29 g NH 4 ReO 4 , 1.93 g of β-cyclodextrin precursor liquid. The precipitating agent used is 4mol / L KOH solution. Add the precursor liquid and the precipitating agent dropwise to the above suspension at a rate of 1 mL / min at the same time, keep the pH value at 9 until the precipitation is complete, wash the precipitate with deionized water until neutral, filter, dry in the air, and dry at 120°C 4 hours, 500°C roasting for 6 hours, the heating rate is 2°C / min.

[0089] Weigh 4g of the above-mentioned catalyst (100 mesh) and place it in the middle of the fixed bed reactor, and fill the remaining space of the reactor with quartz sand. The catalyst activation conditions are: 0.1MP...

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PUM

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Abstract

The invention discloses a method for preparing polyether amine by hydroamination of polyether polyol, a catalyst in the method is mainly composed of a multi-metal active component, an auxiliary agent and a carrier, the multi-metal active component comprises M1-M2 (M1 is one or more than two of transition metals Ni, Co and Cu, and M2 is one or two of transition metals Re and Ru). The catalyst may also comprise an auxiliary agent, and the auxiliary agent is one or a combination of Fe, Cr, Mn, B, Mg, Ba, Pt and other metals or oxides. The catalyst disclosed by the invention is characterized in that in the preparation process of the catalyst, a complexing agent or a stabilizing agent needs to be added into the prepared precursor liquid of the multi-element metal active component and the auxiliary agent so as to improve the catalytic performance. When the catalyst is used for preparing polyether amine through polyether polyol hydroamination, the conversion rate is high, the catalytic performance is stable, the target product selectivity is high, the technological process is simple, the catalyst is suitable for a continuous or batch reactor, and the market prospect is wide.

Description

technical field [0001] The present invention relates to a method for preparing polyether amine by hydrogenation amination of polyether polyol, and relates in detail to a method for preparing polyether polyol and amine in a reactor under certain temperature, pressure and hydrogenation conditions. Chemical agent as raw material, the main production of polyether amine catalyst. Background technique [0002] Polyether amine, also known as amino-terminated polyether, is a kind of polymer whose main chain is polyether structure and the terminal functional group is amine group. Common polyether amines include polyoxyethylene diamine, polyoxypropylene diamine, polyoxyethylene-oxypropylene diamine, polytetramethylene ether diamine, etc. Polyetheramine has excellent reactivity, toughness, viscosity, weather resistance and other properties. As an important fine chemical intermediate, it is widely used in the production fields of polyurethane, epoxy resin curing agent, gasoline deterge...

Claims

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Application Information

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IPC IPC(8): C08G65/325B01J23/889B01J23/89C07C213/02C07C217/08
CPCC08G65/3255B01J23/8896B01J23/8926B01J23/8986B01J23/892C07C213/02C07C217/08
Inventor 马雷丁云杰严丽程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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