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Preparation process of amine terminated polyether

The technology of an amino-terminated polyether and a preparation process is applied in the field of preparation technology of polymer amino-terminated polyether, which can solve the problems of many side reactions, easy self-polymerization of acrylonitrile, difficult operation, etc., and achieves less environmental pollution and convenient post-processing. , selective effect

Inactive Publication Date: 2012-04-11
CHINA PETROCHEMICAL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process route of this method is simple, but in the reaction process of polyether polyol and acrylonitrile, there are many side reactions, and acrylonitrile is easy to self-polymerize, so the requirements for reaction conditions are strict, and the actual operation is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Make 2 times of NaOH into a 20% aqueous solution, put it into a stainless steel three-neck flask equipped with a thermometer, cool it to 50°C with running water, and add Ni-Al alloy powder with a specific mass composition in batches under vigorous stirring Among them (2~4g each time), add within 25~30min. Adjust the speed of adding the alloy so that the temperature of the liquid is kept around 50°C. After the feeding is completed, react at about 80°C for about 90 minutes while stirring. After the production of hydrogen is completed and the mixture is still, the white flocculent reaction product in the upper layer is separated, and the precipitated black Raney nickel catalyst is moved to a beaker, and washed with water until the lotion is neutral to litmus. Then wash with 95% ethanol and absolute ethanol for 2 to 3 times respectively, and finally put them in a container with a closed stopper in absolute ethanol.

Embodiment 2

[0052] Add 100 g of hydroxyl-terminated polyoxypropylene ether with a number average molecular weight of 230.8 and a functionality of 2 (polyether department of Tianjin Petrochemical Co., Ltd.) into a 0.5 L autoclave, and 5 g of a quaternary framework nickel catalyst. Replace the reactor with 0.4MPa nitrogen and hydrogen respectively for 2 to 3 times, pour about 50L of ammonia into the reactor under stirring (under standard conditions), adjust the outlet pressure of the hydrogen cylinder to 2.5MPa, and fill the reactor with hydrogen When the pressure is balanced, the temperature is raised by heating, and the reaction temperature is controlled at 200° C., the reaction time is 4 hours, and the maximum reaction pressure is 14.5 MPa. After the reaction, pass cooling water until the temperature of the reactor is 50°C, slowly exhaust, the gas is absorbed by the secondary water, and the material is discharged.

[0053] Filter the reaction solution while it is hot to separate the cata...

Embodiment 3

[0055] Add 100g of hydroxyl-terminated polyoxypropylene ether with a number-average molecular weight of 230.8 and a functionality of 2 (polyether department of Tianjin Petrochemical Co., Ltd.) into a 0.5L autoclave, and 10g of a quaternary framework nickel catalyst. Replace the reactor with 0.4MPa nitrogen and hydrogen respectively for 2 to 3 times, pour about 50L of ammonia into the reactor under stirring (under standard conditions), adjust the outlet pressure of the hydrogen cylinder to 2.5MPa, and fill the reactor with hydrogen When the pressure is balanced, the temperature is raised by heating, and the reaction temperature is controlled at 200° C., the reaction time is 3 hours, and the maximum reaction pressure is 13.6 MPa. After the reaction, pass cooling water until the temperature of the reactor is 50°C, slowly exhaust, the gas is absorbed by the secondary water, and the material is discharged.

[0056] Filter the reaction solution while it is hot to separate the cataly...

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PUM

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Abstract

The invention belongs to the technical field of polymer materials and provides a preparation process of amine terminated polyether. In the process, polyether polyol with a number-average molecular weight of more than 100 is used as a raw material, and polyetheramine is prepared by catalytic reduction and amination in the presence of hydrogen, an aminating agent and a skeleton nickel catalyst, wherein the skeleton nickel catalyst comprises the following components by mass percent: 80-95% of metal nickel, 5-20% of metal aluminum and 0.5-5% of one, two or three of chromium, iron, copper or zinc; and the skeleton nickel catalyst and the aminating agent can be circularly applied after being processed. The whole preparation process has the advantages of good route selectivity, high conversion rate, low environmental pollution, and convenience in posttreatment.

Description

technical field [0001] The invention belongs to the field of polymer materials and relates to a preparation process of polymer amino-terminated polyether. Background technique [0002] Amino-terminated polyether is a kind of compound with soft polyether skeleton and terminal end capped with amino group or amino group. Most of these compounds are obtained by chemically treating terminal hydroxyl groups with corresponding polyether polyols as raw materials. According to the structure of the hydrocarbon group connected to the terminal amino group, it can be divided into two types: aromatic and aliphatic. At present, amino-terminated polyether is used as curing agent, adhesive, polyurethane and spray polyurea elastomer (SPUA for short) raw material of epoxy resin, in anticorrosion, pipeline, construction, ship, water conservancy, transportation, machinery, It has been widely used in fields such as mine wear resistance. There are three main synthesis methods for amino-terminate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00C08G65/325C08G65/333B01J25/02
Inventor 储政袁俊秀徐冬梅王康金刚
Owner CHINA PETROCHEMICAL CORP
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