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A kind of preparation method of amino-terminated polyether

A technology of amino-terminated polyether and amino polyether, which is applied in the field of preparation of large-molecular-weight polyether, can solve the problems of high preparation cost, harsh preparation conditions, ammonia and hydrogen pollution of the environment, and achieve low reaction temperature and pressure, polymerization The effect of controllable degree and low impurity content

Active Publication Date: 2015-12-23
NANJING BOTE BUILDING MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of the unsatisfactory ammoniation effect in the preparation of amino-terminated polyether in the prior art, resulting in unstable product performance, environmental pollution by residual ammonia and hydrogen; and the problem that its preparation conditions are relatively harsh, resulting in high preparation costs, the present invention provides A kind of preparation method of amino-terminated polyether

Method used

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  • A kind of preparation method of amino-terminated polyether
  • A kind of preparation method of amino-terminated polyether

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Embodiment 1

[0048] Synthesis of single-ended amino polyether products with a degree of polymerization of isopropyl oxirane of 20. Initiator NaOH (as a catalyst at the same time); cycloethylamine is an end-capping agent, and the amount used is the same as the number of moles of NaOH. Weigh 40.00Kg of NaOH and add it into the reaction kettle, and vacuumize to -0.1MPa. Then the temperature of the reaction kettle is raised to 80°C, and 1720.00Kg of isopropyl oxirane is passed into the reaction kettle within 1 hour, and the temperature of the reaction kettle is maintained between 80°C and 90°C and the pressure is between 1.5MPa and 2Mpa during the feeding process. , After the addition of isopropyl oxirane, keep the temperature at 80°C for about 1h. Until the pressure of the reactor no longer decreases, vacuumize to -0.1MPa, and then feed 43.00Kg of cycloethylamine into the reactor. When the pressure in the reactor no longer decreases, it means that the reaction has ended. Release the materia...

Embodiment 2

[0050] Synthesis of single-ended amino polyether products with a polymerization degree of butyl oxirane of 20. Initiator KOH (as a catalyst at the same time); Cycloethylamine is an end-capping agent, and the amount used is the same as the number of moles of KOH. Weigh 56.00Kg of KOH into the reaction kettle, and vacuumize to -0.1MPa. Then the temperature of the reaction kettle is raised to 120°C, and 2000.00Kg of butyl ethylene oxide is introduced into the reaction kettle within 0.5h. After the addition of ethane, keep the temperature at 120°C for about 5 hours. Until the pressure of the reactor no longer drops, vacuumize to -0.1MPa. Then feed cycloethylamine 43.00Kg in the reactor, and when the pressure in the reactor no longer decreased, the reaction had ended. Release the material in the reaction kettle, which is dark brown and has a strong ammonia smell, and the ammoniation rate of the aforementioned material is tested.

Embodiment 3

[0052] Synthesis of single-ended amino polyether products with a degree of polymerization of ethylene oxide of 40. Initiator sodium methoxide (as a catalyst at the same time); cycloethylamine is an end-capping agent, and the consumption is the same as the molar number of sodium methoxide. Weigh 54.00Kg of sodium methoxide into the reaction kettle, and vacuumize to -0.1MPa. Then the temperature of the reaction kettle is raised to 100°C, and 1760.00Kg of ethylene oxide is introduced into the reaction kettle within 3 hours. After the addition of ethane, keep the temperature at 100°C for about 1 hour. Until the pressure of the reactor no longer drops, vacuumize to -0.1MPa. Then feed cycloethylamine 43.00Kg in the reactor, and when the pressure in the reactor no longer decreased, the reaction had ended. Release the material in the reaction kettle, which is light brown and has a strong ammonia smell, and the ammoniation rate of the aforementioned material is tested.

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Abstract

The invention provides a preparation method of amine-terminated polyether. The preparation method is characterized in that the amine-terminated polyether is prepared by using the ring-opening reaction of cyclo-nitrogen alkane and epoxyalkane, wherein the temperature of the reaction system is 80-120 DEG C, and the pressure of the reaction system is 0.2-10 MPa. The degree of polymerization of the obtained amine-terminated polyether is controllable, and the ammoniation rate is high; compared with a catalytic reduction ammoniation method, the preparation method has the advantages that the reaction temperature and pressure are lower, and product post-treatment does not need filtration, ammonia gas removal and the like.

Description

technical field [0001] The invention relates to a method for preparing a large molecular weight polyether, in particular to a method for preparing an aliphatic amino-terminated polyether. Background technique [0002] Amine-Terminated Polyether (ATPE for short), also known as polyether amine, is a type of polyoxyalkylene compound capped by a primary or secondary amino group. The terminal amino group of its macromolecular chain contains active hydrogen, which can react with groups such as isocyanate groups and epoxy groups, and is an important raw material for the synthesis of various chemical products. For example, reaction injection molding (RIM) polyurea and spray polyurea elastomer (SPUA), used as anti-turbidity and anti-sedimentation additives in engine fuel, curing crosslinking agent for epoxy resin, etc. [0003] Amino-terminated polyether can be divided into monoamino polyether, diamino polyether and triamino polyether series according to the number of terminal amino...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/333C08G65/28C07C217/08C07C213/02
Inventor 冉千平范士敏王涛吕志峰杨勇张志勇吴井志
Owner NANJING BOTE BUILDING MATERIALS CO LTD
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