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Process of producing small molecular weight polyether amine by continuous method

A low-molecular-weight, polyetheramine technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of high process conditions, limited yield, decreased catalyst activity, etc., and achieves simple process steps. , the effect of increasing production and reducing impact

Active Publication Date: 2014-10-29
WUXI ACRYL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production equipment is complex and the process conditions are high
Especially in the production of low-molecular-weight polyetheramine, due to the high water content generated by the reaction, the catalyst activity will decrease rapidly in the continuous production process. The requirements for the catalyst used are very high, and the output is also limited.
[0008] At present, the polyetheramine continuous production process in the world adopts a single catalyst system and a single reactor. When producing polyetheramine with a small molecular weight, the proportion of water generated is high, which will easily cause the activity of the catalyst to decrease and limit the output. The invention adopts a multi-reactor fixed-bed polyetheramine continuous production process, and uses different catalyst systems in each reactor

Method used

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  • Process of producing small molecular weight polyether amine by continuous method
  • Process of producing small molecular weight polyether amine by continuous method

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Experimental program
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Effect test

Embodiment 1

[0019] The reaction was carried out in a fixed-bed reactor with continuous feeding, and the reactor included 4 tubular reactors connected in series. The inner diameter of the tubular reactor was 13mm, and each reactor was filled with 100ml of catalyst.

[0020] The tubular reactors are filled with the following catalysts from front to back, the first reactor: Raney metal catalyst, the metal nickel content is 100%, the average particle size is 3mm; the second reactor: the supported metal with alumina as the carrier Catalyst, the particle size is 3mm * 3mm, the loaded metal content (reduction state) is, nickel 30%, copper 10%; The third reactor: the metal supported catalyst with alumina as the carrier, the particle size is 3mm * 3mm, the load The metal content (reduced state) is 25% nickel, 15% copper, and 1.5% chromium; the fourth reactor: a metal-supported catalyst with alumina as a carrier, the particle size is 3mm×3mm, and the loaded metal content (reduced state) For, nickel...

Embodiment 2

[0025] The experimental device is the same as that of Example 1, and the same catalysts are filled in the 4 reactors, all of which are Raney metal catalysts, the metal content is 100% nickel, and the average particle size is 3mm.

[0026] The reaction temperature is 220°C, and the reaction pressure is 13.5Mpa.

[0027] The polyether used is polypropylene glycol ether with an average molecular weight of 230. Liquid ammonia and polyether hydroxyl are mixed at a molar ratio of 60:1, and enter the reactor through a liquid feed pump at a feed rate of 600 g / h and a hydrogen flow rate of 0.45 liter / min.

[0028] Table 1 lists the total amine values ​​of the products obtained at different times after the feed is deaminated and dehydrated.

Embodiment 3

[0030] Experimental apparatus is identical with embodiment one, fills identical catalyst in 4 reactors, is the metal supported catalyst that is carrier with alumina, and particle diameter is 3mm * 3mm, and loaded metal content (reduced state) is: nickel 20%, Copper 18%, Ruthenium 1.5%.

[0031] The reaction temperature is 220°C, and the reaction pressure is 13.5Mpa.

[0032] The polyether used is polypropylene glycol ether with an average molecular weight of 230. Liquid ammonia and polyether hydroxyl are mixed according to the molar ratio of 60:1, and then enter the reactor sequentially through the liquid feed pump. 1.25:1.

[0033] Table 1 lists the total amine values ​​of the products obtained at different times after the feed is deaminated and dehydrated.

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Abstract

The invention relates to a process of producing small molecular weight polyether amine by a continuous method. A continuous method fixed bed process is adopted, polyether, liquid ammonia and hydrogen are used as raw materials, 2-6 reactors which are fixed bed reactors or tubular reactors are connected in series and each reactor is internally filled by a Raney metal catalyst or a supported metal catalyst, respectively; under the reaction condition of certain temperature, pressure and molar proportion, the raw materials are sequentially reacted through the reactors to obtain polyether amine, the molecular weight of which is 100-1000. The process provided by the invention is simple in step. Multiple reactors and a compound catalyst system are adopted, so that the influence of generated water in the reaction to the catalyst efficiency is effectively reduced, and the yield and the conversion ratio of reaction are improved.

Description

technical field [0001] The invention relates to a preparation method of polyetheramine, in particular to a continuous method for producing low-molecular-weight polyetheramine, which belongs to the technical field of polymer synthesis and preparation. Background technique [0002] Polyetheramine is a kind of compound with polyoxyalkylene structure as the main chain and amine group as the active functional group. Because of its special structure, it is widely used in many fields. There are many ways to introduce amine groups at the end of polyether, but at present, the real large-scale industrial production is mainly the catalytic amination of hydroxyl groups at the end of polyether under the action of metal catalysts. [0003] The catalytic amination of polyether hydroxyl can adopt two kinds of production processes, continuous method and batch method. [0004] CN1546550A discloses that under the action of a Raney nickel metal catalyst, amino polyether is prepared from polye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/08C07C213/02C08G65/325
Inventor 张文泉尤卫民朱萌朱学军潘萍施英范慧军
Owner WUXI ACRYL TECH
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