Continuous preparation method of amine-terminated polyether

A technology of amino-terminated polyether and polyether polyol, which is applied in the field of polymer chemistry, can solve the problems of polluting polyether polyol and polyether amine with many side reactions and difficult gasification, and achieve high primary amine selectivity and operation The effect of continuous process and solution to the decline of conversion rate

Active Publication Date: 2014-12-24
HONGBAOLI GRP CO LTD +1
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Problems solved by technology

[0010] Purpose of the invention: The purpose of the present invention is to overcome the many side reactions, harsh conditions, serious pollution of the existing batch method for preparing polyetheramine, and the difficulty of gasification of large molecular weight polyether polyols and NH in the existing continuous preparation of amino-terminated polyether methods. 3 and H 2 It does not reuse the disadvantages of polluting the environment, and provides a method for the continuous preparation of amino-terminated polyethers under relatively mild conditions, which is easy to operate

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  • Continuous preparation method of amine-terminated polyether

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Embodiment 1

[0036] 10mL of hydroamination catalyst (containing Ni 92%, Co 3%, Cr 3%, Mo 2%) was filled in In a fixed-bed reactor (20 mm in diameter, 320 mm in height, and about 100 ml in volume), the raw material polyether polyol is preheated to 50° C. Continuously press 2.0MPa constant pressure H into the reactor at a flow rate of 30L / h 2 , the volume space velocity is 1.4h-1 NH 3 and a volumetric space velocity of 5.0h -1 , molecular weight 230, functionality of 2 raw material polyether polyol (NH 3 The ratio of the number of moles to the number of moles of hydroxyl groups in polyether polyol molecules is 1:1; H 2 The ratio of the number of moles to the number of moles of hydroxyl groups in the polyether polyol molecule is about 3:1); polyether, NH 3 and H 2 After being atomized by the atomizer at the top of the reactor, it contacts with the hydroammination catalyst filled in the middle of the reactor, and the hydroammination reaction occurs at 190°C and 13.0MPa, and the product p...

Embodiment 2

[0039] 30mL of hydroamination catalyst (containing 91% Ni, 4% Co, 3.5% Cr, 1.5% Mo) was filled in the above-mentioned fixed-bed reactor, and the raw material polyether polyol was preheated to 60°C. Continuously press 1.5MPa constant pressure H into the reactor at a flow rate of 25L / h 2 , the volume space velocity is 0.47h -1 NH 3 and a volumetric space velocity of 1.5h -1 , a raw material polyether polyol with a molecular weight of 400 and a functionality of 2 (NH 3 The ratio of the number of moles to the number of moles of hydroxyl groups in polyether polyol molecules is 2:1; H 2 The ratio of the number of moles to the number of moles of hydroxyl groups in the polyether polyol molecule is about 4:1). Polyether, NH 3 and H 2 After being atomized by the atomizer at the top of the reactor, it contacts with the hydroammination catalyst filled in the middle of the reactor, and the hydroammination reaction occurs at 200°C and 11.0MPa, and the product is separated at 130°C by ...

Embodiment 3

[0042] 50mL of hydroamination catalyst (containing Ni 92%, Co 2%, Cr 5%, Mo 1%) was filled in the above-mentioned fixed-bed reactor, and the raw material polyether polyol was preheated to 110°C. Continuously pressurize 1.0MPa constant pressure H into the reactor at a flow rate of 15L / h 2 , the volume space velocity is 0.35h -1 NH 3 and a volumetric space velocity of 0.8h -1 , the molecular weight is 1000, the raw material polyether polyol (NH 3 The ratio of the number of moles to the number of moles of hydroxyl groups in polyether polyol molecules is 7:1; H 2 The ratio of the number of moles to the number of moles of hydroxyl groups in the polyether polyol molecule is about 6:1). Polyether, NH 3 and H 2 After being atomized by the atomizer at the top of the reactor, it contacts with the hydroammination catalyst filled in the middle of the reactor, and the hydroammination reaction occurs at 210°C and 9.7MPa, and the product passes through the primary and secondary gas-liq...

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Abstract

The invention discloses a continuous preparation method of amine-terminated polyether, and the method comprises the following steps of: taking polyether polyol, H2 and NH3 as raw materials, executing critical hydroamination in a fixed bed reactor under a critical hydroamination catalyst, executing gas-liquid separation in a gas-liquid separator to feed liquid from the fixed bed reactor, reusing NH3 and H2 without being reacted after being dried and pressurized; accessing the liquid material into a vacuum chamber, removing H2O and other small-molecule materials in vacuum, continuously discharging to prepare amine-terminated polyether. The method is continuous in operating processes and more steady in a product quality batch method; in preparation, the gas can be reused to prevent environmental pollution; the method can effectively solve the problems of decreased conversion and weak selectivity caused by poorly contacting the gas and the catalyst during large-molecular polyether reaction; the method has the advantages of higher reaction conversion ratio and primary amine selectivity.

Description

technical field [0001] The invention belongs to the technical field of polymer chemistry, and mainly relates to a continuous preparation method of amino-terminated polyether. Background technique [0002] Amine-Terminated Polyether (ATPE), also known as polyether amine, is a kind of polyoxyalkylene compound, the main chain of which is a polyether skeleton, but the end is blocked by an amino group. According to the number of substituted H atoms in the amino group, it can be divided into primary amino group and secondary amino group terminated amino polyether. At present, the international market of amino-terminated polyether products is mainly monopolized by Huntsman and Basf. There are only a few companies in China that can produce them, but most of them are batch methods, and the product quality is unstable. Their production capacity cannot meet the needs of the domestic market at all. [0003] At present, the synthesis methods of known amino-terminated polyethers include:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00
Inventor 沈小勇邢益辉唐黎余渡江
Owner HONGBAOLI GRP CO LTD
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