Continuous preparation device of small molecular weight amine-terminated polyether and preparation method

A technology of amino-terminated polyether and small molecular weight, which is applied in the preparation of amino-hydroxyl compounds, the preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of low primary amine content and poor product quality, and achieve low reaction temperature and pressure , increase economic benefits and reduce usage

Pending Publication Date: 2018-04-06
HONGBAOLI GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The primary amine selectivity of the amino-terminated polyether product synthesized by this method is greater than 95%, and the reaction conversion rate is also greater than 95%, but the H in the reaction process cannot be realized. 2 and liquid NH 3 and the content of primary amine in the product is lower than that of domestic related products, and the product quality is poor

Method used

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  • Continuous preparation device of small molecular weight amine-terminated polyether and preparation method

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Embodiment 1

[0053] 100mL supported nickel-based catalyst (containing Ni 92%, Cr 7.8%, Fe 0.2%) and 100mL Raney-type nickel-based catalyst (particle size 20 mesh, activity 1ml H 2 / min. g) Fill in fixed-bed reactors I and II of φ25×720mm (diameter 25mm, height 720mm, volume about 350ml) (catalyst volume to fixed bed volume ratio is 0.29:1), heat up and feed H 2 Activate and dry. After completion, press H into the mixing preheater at a flow rate of 12L / h 2 , the volume space velocity is 2.0h -1 NH 3 and a volumetric space velocity of 1.0h -1 , molecular weight 230, low molecular weight polyether (NH 3 The molar ratio to the hydroxyl group in the polyether polyol molecule is 8:1; H 2 The molar ratio to the hydroxyl group in the polyether polyol molecule is about 0.6:1); fully mixed and preheated at 60°C, and then enters the fixed bed reactor I from the top, and the first step of hydrogenation occurs at 180°C and 2.5MPa Ammonification reaction: the product is separated from gas and liq...

Embodiment 2

[0056] 35mL supported nickel-based catalyst (containing Ni 95%, Cr 3%, Fe 2%) and 35mL Raney-type nickel-based catalyst (particle size 40 mesh, activity 5ml H 2 / min. g) Fill in fixed bed reactors I and II of φ25×720mm (diameter 25mm, height 720mm, volume 350ml) (catalyst volume to fixed bed volume ratio is 0.2:1), heat up and feed H 2 Activate and dry. After completion, press H into the mixing preheater at a flow rate of 8L / h 2 , the volume space velocity is 4.0h -1 NH 3 and a volumetric space velocity of 2.0h -1 , molecular weight 400, low molecular weight polyether (NH 3 The molar ratio to the hydroxyl group in the polyether polyol molecule is 15:1; H 2 The molar ratio to the hydroxyl group in the polyether polyol molecule is about 1:1); fully mixed and preheated at 50°C, and then enters the fixed bed reactor I from the top, and the first step of hydrogenation occurs at 140°C and 1.5MPa Ammonification reaction: the product is separated from gas and liquid at 160°C by...

Embodiment 3

[0059] 155mL supported nickel-based catalyst (containing Ni 90%, Cr 8%, Fe 2%) and 155mL Raney-type nickel-based catalyst (particle size 30 mesh, activity 3ml H 2 / min. g) Fill in fixed bed reactors I and II of φ25×720mm (diameter 25mm, height 720mm, volume 350ml) (the ratio of catalyst volume to fixed bed volume is 0.44:1), heat up and feed H 2 Activate and dry. After completion, press H into the mixing preheater at a flow rate of 20L / h 2 , the volume space velocity is 1.0h -1 NH 3 and a volumetric space velocity of 2.0h -1 , a molecular weight of 600, a small molecular weight polyether with a functionality of 2 (NH 3 The molar ratio to the hydroxyl group in the polyether polyol molecule is 5:1; H 2 The molar ratio to the hydroxyl group in the polyether polyol molecule is about 0.9:1); fully mixed and preheated at 100°C, and then enters the fixed bed reactor I from the top, and the first step of hydrogenation occurs at 160°C and 2.0MPa Ammonification reaction: the prod...

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Abstract

The invention discloses a continuous preparation device and preparation method of small molecular weight amino-terminated polyether. A continuous preparation device for small-molecular-weight amino-terminated polyether, including a hydrogen storage device, a liquid ammonia storage tank, a polyether polyol storage tank, a mixing preheater, a fixed-bed reactor I, a fixed-bed reactor II, a primary gas liquid separator, intermediate drying tower, secondary gas-liquid separator, circulating hydrogen compressor, flash deamination tower, pressurized liquefaction device, dehydration tower, waste water pool and product storage tank; , H2 and liquid NH3 are used as raw materials, under the action of a catalyst, two fixed-bed reactors are connected in series, and a "two-step" hydrogenation reaction occurs to prepare a small molecular weight amino-terminated polyether. The invention has continuous operation process, stable and controllable product quality, and mild reaction conditions; the recycling of H2 and liquid NH3 is realized, which is more environmentally friendly and economical; the reaction conversion rate is ≥ 99.0%, and the selectivity of primary amines is ≥ 98.5%.

Description

technical field [0001] The invention relates to a continuous preparation device and method for small-molecular-weight amino-terminated polyethers, belonging to the field of preparation of amino-terminated polyethers. 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 production of domestic amino-terminated polyether products is mostly batch method, with incomplete product types and unstable quality, and the production capacity cannot meet market demand at all. [0003] At present, the synthesis of amino-terminated polyether in foreign companies is mainly a continuous gas, liquid, and solid three-phase fixed-bed hydrogenation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00C07C213/02C07C217/28
CPCC08G65/00C07C213/02C08G2650/04C08G2650/50C07C217/28
Inventor 邢益辉沈小勇黄书宇赵翔
Owner HONGBAOLI GRP CO LTD
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