Method for preparing polyether amine through normal pressure catalysis

A technology for catalytic preparation and polyetheramine, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., which can solve the problems of high equipment investment, operation and maintenance costs and unfavorable Expansion of large-scale production, unfavorable normal safe production, etc., to achieve the effect of high reaction conversion rate and selectivity, reduced reaction difficulty, and convenient maintenance

Active Publication Date: 2017-06-13
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Strict equipment safety requirements, high equipment investment, operation and maintenance costs, are not conducive to industrial scale-up production
In addition, ammonia gas is easy to corrode. Both ammonia gas and hydrogen gas are flammable and explosive gases. Safety accidents are prone to occur under high temperature and high pressure, which is also quite unfavorable for maintaining normal and safe production.

Method used

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  • Method for preparing polyether amine through normal pressure catalysis
  • Method for preparing polyether amine through normal pressure catalysis
  • Method for preparing polyether amine through normal pressure catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Effect of Different Catalyst Systems

[0020] Weigh 100g γ-Al 2 o 3 As a benchmark, metal salts of different weights (see Table 1) and a slightly excessive amount of precipitant sodium carbonate were weighed in 4 different mass ratios and dissolved in an appropriate amount of deionized water of the same volume to form a solution. Add several solutions dropwise to the flask of the stirring device at the same time, and maintain the pH value of the solution at about 9 during the whole dropping process. After the dropwise addition, keep stirring until the precipitation is complete, and let it stand for aging. Then suction filter and wash the filter cake with deionized water, repeat the above steps until there is no nitrate ion. The filter cake was dried in an oven at 120°C and crushed, mixed with an appropriate amount of γ-Al 2 o 3 The powder and binder are evenly ground, extruded into cylindrical strips with an extruder, dried in an oven at 120°C and then r...

Embodiment 2

[0026] Embodiment 2: the influence of temperature of reaction

[0027] The preparation process and working principle of the catalyst in this example are the same as those in Example 1, except that the effect of catalytic amination to prepare polyetheramine at different reaction temperatures is shown in Table 2. Other reaction conditions: polyether (M=980), polyether space velocity 1.5g / h / g / cat, the feed rate (mol / min) of polyether and the feed rate (mol / min) of liquid ammonia, hydrogen The ratio of the feed rate (mol / min) is 1:6:6, and the specific results are shown in Table 2.

[0028] Table 2 Influence of reaction temperature on catalytic amination effect of polyetheramine.

[0029] temperature °C Conversion rates% selectivity% Yield % 170 77.4 75.8 58.7 180 80.5 79.0 63.6 190 83.8 81.9 68.6 200 85.2 83.5 71.1 210 87.5 80.0 70.0 220 90.7 75.1 68.1

[0030] The reaction temperature has a significant impact on the ...

Embodiment 3

[0031] Example 3: Effect of Hydrogen Feed Rate

[0032] The preparation process and working principle of the catalyst in this example are the same as those in Example 1, the difference is that the effect of catalytic amination to prepare polyetheramine at different hydrogen feed rates is shown in Table 3. Other reaction conditions: polyether (M=980), reaction temperature 200 ℃, polyether space velocity 1.5g / h / g / cat, the feed rate of polyether (mol / min) the feed rate of ammonia gas (mol / min) ratio is 1:6, the specific results are shown in Table 3.

[0033] Table 3 The effect of the amount of hydrogen on the catalytic amination effect of polyetheramine.

[0034] n(polyether:H 2 )

[0035] Polyether catalyzed amination has both dehydrogenation and hydrogenation processes. If the amount of hydrogen is too low, the reaction cannot be carried out normally, and if it is too high, the reaction will be reversed. From the perspective of chemical balance, in polyether: H ...

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Abstract

The invention relates to a method for preparing polyether amine through normal pressure catalysis, and belongs to the technical field of organic high-molecular compound preparation or chemical processing. Polyoxyethylene ether, liquid ammonia and hydrogen gas are used as raw materials; the raw materials are introduced into a tubular fixed bed reactor filled with catalysts; the reaction temperature is controlled at 160 to 210 DEG C; the polyether air speed is 0.1 to 4 g / h / g / cat; the ratio of the feeding speed rate of the polyether to the feeding speed rate of liquid ammonia to the feeding speed rate of the hydrogen gas is 1:(3 to 12):(3 to 12); after the reaction is completed, filtering is performed to obtain the polyether amine product. When the method is applied to the polyether amine production, the advantages of mild reaction condition, high controllability and the like are realized.

Description

technical field [0001] The invention relates to a method for catalytically preparing polyetheramine under normal pressure, and belongs to the technical field of preparation or chemical processing of organic polymer compounds. Background technique [0002] Polyether Amine (PEA) is a kind of polyolefin compound with soft polyether backbone and terminated by primary or secondary amino groups. Most polyetheramines are obtained from the corresponding polyether polyols as raw materials by amination of terminal hydroxyl groups. According to the type of hydrocarbon groups connected to the terminal amino groups, they can be divided into two types: aromatic and aliphatic. The main chain of polyetheramine molecule is a soft polyether chain, and the hydrogen on the terminal is more active than the hydrogen on the terminal hydroxyl group of polyether. Therefore, polyetheramine can replace polyether very well in some materials and processes, and can improve new The application performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/325B01J23/44B01J23/58B01J23/63
CPCB01J23/44B01J23/58B01J23/63C08G65/3255C08G2650/10C08G2650/50
Inventor 余江金一丰尹红王月芬宋明贵万庆梅
Owner ZHEJIANG HUANGMA TECH
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