Continuous production method for amino end-capped polyether

A technology of amino-terminated polyether and its production method, which is applied in chemical instruments and methods, preparation of amino hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of low mass transfer and heat transfer efficiency, unstable quality, high reaction pressure, etc. Achieve the effects of improving production efficiency and product conversion rate, high mass and heat transfer efficiency, and mild reaction conditions

Active Publication Date: 2012-07-18
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a continuous production method of amino-terminated polyether, which solves the problems of small contact area between reaction mediums, low efficiency of mass transfer and heat transfer, high reaction pressure, many side reactions, etc. Low production efficiency, unstable quality, poor safety and reliability, etc., realize continuous production of amino-terminated polyether from hydroxyl-terminated polyether

Method used

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  • Continuous production method for amino end-capped polyether
  • Continuous production method for amino end-capped polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] use figure 1 The shown continuous reaction device carries out the following operation process. Add polyethylene glycol with a molecular weight of 1000 to the polyether drying treatment device 1, stir and raise the temperature to 120°C, continue vacuuming to above -0.09MPa, and continue dehydration for 4 hours, then transfer the material to the temporary storage tank 2. Inject 200kg of polyether and 34kg of liquid ammonia into the mixer 3 in two batches from the polyether temporary storage tank, and inject 0.08kg of hydrogen at an initial pressure of 2MPa. Then mix the material at a space velocity of 1.8h -1Feed material is heated by the heating device 4 and enters the tubular reactor 5 filled with macroporous nickel-based catalyst carrier. The reaction temperature is maintained at 180-200°C, the reaction pressure is 10-11MPa, and the reaction is continued for 80 hours. After the material undergoes continuous catalytic reaction in the tubular reactor, it is cooled to 1...

Embodiment 2

[0030] use figure 1 The shown continuous reaction device carries out the following operation process. Add polypropylene glycol with a molecular weight of 400 to the polyether drying treatment device 1, stir and raise the temperature to 140°C, continue vacuuming to above -0.09MPa, and continue dehydration for 5 hours, then transfer the material to the temporary storage tank 2. Inject 100kg of polyether and 85kg of liquid ammonia into the mixer 3 in two batches from the polyether temporary storage tank, and inject 2kg of hydrogen at an initial pressure of 5MPa. Then mix the material at a space velocity of 0.08h -1 The feed material is heated by the heating device 4 and then enters the tubular reactor 5 filled with a macroporous nickel-based catalyst carrier. The reaction temperature is maintained at 240~260°C, the reaction pressure is 12~13MPa, and the reaction is continued for 50h. After the material undergoes continuous catalytic reaction in the tubular reactor, it is co...

Embodiment 3

[0032] use figure 1 The shown continuous reaction device carries out the following operation process. Add polyoxypropylene triol with a molecular weight of 3000 to the polyether drying treatment device 1, stir and raise the temperature to 130°C, continue vacuuming to above -0.09MPa, and continue dehydration for 6 hours, then transfer the material to the temporary storage tank 2. Inject 300kg of polyether and 255kg of liquid ammonia into the mixer 3 in two batches from the polyether temporary storage tank, and inject 3kg of hydrogen at an initial pressure of 3MPa. Then mix the material at a space velocity of 1.1h -1 The feed material is heated by the heating device 4 and then enters the tubular reactor 5 filled with a macroporous nickel-based catalyst carrier. The reaction temperature is maintained at 200-220 ° C, the reaction pressure is 11-12 MPa, and the reaction is continued for 80 hours. After the material undergoes continuous catalytic reaction in the tubular reactor, i...

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Abstract

The invention relates to a continuous production method for amino end-capped polyether. The method comprises the following three continuous phases of: (1) a pre-treatment phase: dehydrating and drying a polyether raw material, proportionally mixing with hydrogen and liquid ammonia to form a mixed material, and heating to a reaction temperature; (2) a reaction phase: putting the mixed material into a tubular reactor, contacting with a porous nickel-based catalyst filled into the tubular reactor, and undergoing a hydro-ammoniation reaction under the action of the catalyst; and (3) a post-treatment phase: cooling a product generated in the reaction phase, introducing into a gas-liquid separating device, separating ammonia gas and hydrogen gas from a liquid product, filtering the separated liquid, and drying to obtain a finished product. The continuous production method has the advantages of realization of continuous production of aminopolyether, high mass transfer and heat transfer efficiencies, high reaction speed, mild reaction condition, reduction in side reactions, safety and reliability. The catalyzing efficiency of the catalyst is high, and the production efficiency and the conversion rate of the product are effectively increased.

Description

technical field [0001] The invention relates to a continuous production method of amino-terminated polyether, which belongs to the technical field of organic chemical industry. Background technique [0002] Amino-terminated polyether is a kind of polyoxyalkylene compound whose end is composed of primary or secondary amino groups, and belongs to the derivatives of polyether polyol or polyethylene glycol series. Amino-terminated polyether has higher reactivity than hydroxyl-terminated polyether, and has fast reaction speed and high conversion rate with isocyanate groups, epoxy groups, carboxylic acid groups, etc., and has obvious advantages. It is mainly used for Used in lubricating oil additives, synthetic raw materials for high-performance polyurea materials, curing agents for epoxy resins, surfactants and medical materials, etc. [0003] There are three main synthetic methods of amino-terminated polyether reported at home and abroad: 1. Hydrogenation method, that is, h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08G65/325C07C213/02C07C217/08
Inventor 冉千平杨勇刘加平黄玉成周栋梁刘金芝
Owner JIANGSU SOBUTE NEW MATERIALS
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