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A method for preparing polyamines by direct ammoniation of polyhydroxy compounds

A technology of polyhydroxy compounds and polyamines, applied in the preparation of amino hydroxyl compounds, amino compounds, organic compounds, etc., can solve the problems of high pressure, high cost of raw materials, environmental pollution, etc., and achieve good selectivity and reactivity high effect

Active Publication Date: 2018-06-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still some problems in the above process, such as high hydrolysis temperature and high pressure, azide heating and releasing a large amount of nitrogen may cause explosion, high cost of raw materials, environmental pollution and other problems

Method used

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  • A method for preparing polyamines by direct ammoniation of polyhydroxy compounds

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Catalyst A Preparation

[0020] Add 800mL of ethylene glycol, 10g of copper acetate, 50g of powdered ZSM-5 molecular sieve and 50g of deionized water into a 1500mL round-bottomed flask, mechanically stir evenly and raise the temperature to 90°C until the copper acetate is completely dissolved. Add 150mL of NaOH aqueous solution with a mass concentration of 10% to the solution at a high speed. After dripping the lye, stir for 2 hours and slowly heat up to evaporate the water in the system. After cooling down to room temperature, the solid precipitate was filtered out with suction, and washed thoroughly with deionized water, methanol, and acetone to obtain catalyst A for the reaction.

[0021] Amination reaction

[0022] Add 30g of 1,4-butanediol and 4g of the above-mentioned catalyst A into a 100mL autoclave, replace it with nitrogen and raise the temperature to 250°C, pressurize ammonia gas at a pressure of 6Mpa into the autoclave, and continue to pressurize hydrogen g...

Embodiment 2

[0024] Catalyst B Preparation

[0025] Add 800mL of ethylene glycol, 10g of nickel acetate, 50g of powdered ZSM-5 molecular sieve and 50g of deionized water into a 1500mL round-bottomed flask, mechanically stir evenly and raise the temperature to 90°C until the copper acetate is completely dissolved. Drop 150mL of 10% NaOH aqueous solution into the solution at a high speed. After dropping the lye, stir for 2 hours and slowly raise the temperature to evaporate the water in the system. At room temperature, the solid precipitate was filtered out with suction, and washed thoroughly with deionized water, methanol, and acetone to obtain catalyst B for the reaction.

[0026] Amination reaction

[0027] Add 30g of 1,4-butanediol and 4g of the above-mentioned catalyst B into a 100mL autoclave, replace it with nitrogen and raise the temperature to 250°C, pressurize ammonia gas with a pressure of 6Mpa into the autoclave, and continue to pressurize hydrogen gas with a pressure of 8Mpa ,...

Embodiment 3

[0029] Catalyst C Preparation

[0030] Add 800mL of ethylene glycol, 5g of copper acetate, 5g of nickel acetate, 50g of powdered ZSM-5 molecular sieve and 50g of deionized water into a 1500mL round bottom flask, mechanically stir evenly and heat up to 90°C until the copper acetate is completely dissolved. Drop 150mL of 10% NaOH aqueous solution into the solution at a rate of 1mL / min. After dropping the lye, stir for 2 hours and slowly raise the temperature to evaporate the water in the system. When the temperature of the system rises to 180°C, reflux the ethylene glycol for 8 hours , when it was lowered to room temperature, the solid precipitate was filtered out by suction, and then washed thoroughly with deionized water, methanol and acetone to obtain catalyst C for the reaction.

[0031] Amination reaction

[0032] Add 30g of 1,4-butanediol and 4g of the above-mentioned catalyst C into a 100mL autoclave, replace it with nitrogen and program the temperature to 250°C, pressur...

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Abstract

A method for the direct ammoniation of polyols to prepare polyamines, using polyols, ammonia gas or liquid ammonia as raw materials, and the carrier-loaded liquid-phase reduced transition metal as a catalyst, realizing the ammoniation of polyols under milder conditions reaction. The catalyst has high selectivity to polyamines, and the catalyst can be recycled and reused.

Description

technical field [0001] The present invention relates to the presence of a catalyst with Cu and Ni as the main components, through polyol and NH 3 A one-step method for the preparation of polyamines by the hydroammination reaction. Background technique [0002] Polyamines are important basic chemical raw materials, which are widely used as solvents, chelating agents, stabilizers, pharmaceutical intermediates and in the synthesis of polyurethane. [0003] A variety of methods for preparing polyamines have been described in the literature. Taking 1,3-propanediamine as an example, the main preparation methods are the ammonolysis method of halogenated hydrocarbons and the acrylocyanide method. The ammonolysis method of halogenated hydrocarbons (RU 226118; RU 226191) uses 1,3-dichloropropane as raw material to generate 1,3-propanediamine through ammonolysis. The acrylonitrile method mainly prepares 3-aminopropanecyanide by first reacting acrylocyanide with ammonia, and then prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/16C07C211/09C07C211/10C07C211/11C07C213/02C07C215/18B01J29/46B01J29/48B01J23/889
CPCY02P20/50
Inventor 孙颖徐杰高进郑玺杜文强石松
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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