A method of preparing 1,2-diaminopropane from isopropanolamine and liquid ammonia and a device thereof

A technology of isopropanolamine and propylenediamine, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of unfavorable industrial production of the preparation method, low selectivity of 1,2-propylenediamine, Catalyst and product separation difficulties and other problems, to achieve the effect of large-scale continuous industrial production, improve selectivity, reduce one-time investment and production costs

Active Publication Date: 2015-06-10
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

The main problems at present are that the conditions of the reaction are harsh, the tank reaction generally needs to add a solvent, the separation of the catalyst and the product is difficult, the selectivity of 1,2-propanediamine is relatively low, and the preparation method is not conducive to large-scale continuous industrial production

Method used

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  • A method of preparing 1,2-diaminopropane from isopropanolamine and liquid ammonia and a device thereof
  • A method of preparing 1,2-diaminopropane from isopropanolamine and liquid ammonia and a device thereof
  • A method of preparing 1,2-diaminopropane from isopropanolamine and liquid ammonia and a device thereof

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Experimental program
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Embodiment 1

[0050] Weigh the above 15%Ni-1.6%Re-1.2%B / Al 2 O 3 The catalyst, 3.2 grams (about 4 ml), was charged into the fixed bed reactor. The catalyst is activated by hydrogenation before use. The activation conditions are: temperature T=375℃; pressure P=normal pressure, gas volume space velocity GHSV=2000h -1 , the restoration time is 4 hours. When the temperature in the reactor is naturally cooled to 140 °C, the pressure is increased to 8MPa. After the system is stabilized, the liquid ammonia / isopropanolamine = 10 (molar ratio) is pumped into the reactor to adjust the isopropanolamine. The volumetric space velocity of the liquid is 0.5h -1 , the H2 content in the reaction system was 2.5 mol%, the reaction was carried out, the reaction time was 50 hours, and the sample was taken for analysis. SE-30 capillary chromatographic column, FID detector, N,N-dimethylformamide as internal standard for quantitative analysis, the reaction results are shown in Table 1. The product can be dist...

Embodiment 2

[0051] Weigh the above 15%Ni-1.6%Re-1.2%B / Al 2 O 3 The catalyst, 3.2 grams (about 4 ml), was charged into the fixed bed reactor. The catalyst is activated by hydrogenation treatment before use, and the activation conditions are: T=375℃; P=normal pressure, GHSV=2000h -1 , the restoration time is 4 hours. When the temperature in the reactor is naturally cooled to 150 °C, the pressure is increased to 8MPa. After the system is stabilized, the liquid ammonia / isopropanolamine = 10 (molar ratio) is pumped into the reactor to adjust the isopropanolamine. The volumetric space velocity of the liquid is 0.5h -1 , H in the reaction system 2 The content was 2.5 mol%, the reaction was carried out, and the reaction time was 50 hours, and the samples were taken for analysis. SE-30 capillary chromatographic column, FID detector, N,N-dimethylformamide as internal standard for quantitative analysis, the reaction results are shown in Table 1.

Embodiment 3

[0053] Weigh the above 15%Ni-1.6%Re-1.2%B / Al 2 O 3 The catalyst, 3.2 grams (about 4 ml), was charged into the fixed bed reactor. The catalyst is activated by hydrogenation treatment before use, and the activation conditions are: T=375℃; P=normal pressure, GHSV=2000h -1 , the restoration time is 4 hours. When the temperature in the reactor is naturally cooled to 170°C, the pressure is increased to 8MPa. After the system is stabilized, the liquid ammonia / isopropanolamine = 10 (molar ratio) is pumped into the reactor to adjust the isopropanolamine. The volumetric space velocity of the liquid is 0.5h -1 , H in the reaction system 2 The content was 2.5 mol%, the reaction was carried out, and the reaction time was 50 hours, and the samples were taken for analysis. SE-30 capillary chromatographic column, FID detector, N,N-dimethylformamide as internal standard for quantitative analysis, the reaction results are shown in Table 1.

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Abstract

The invention relates to a method of preparing 1,2-diaminopropane from isopropanolamine and liquid ammonia. The method includes mixing the isopropanolamine and the liquid ammonia according to a certain ratio, pumping the mixture into a reactor and reacting under existence of a catalyst and hydrogen. The method adopts the novel catalyst which is excellent in catalytic performance and prone to long-term operation. The method allows production of a diaminopropane product by hydroamination of the isopropanolamine to be achieved under a low reaction pressure. By adjustment of reaction conditions, composition of products can be regulated flexibly and selectivity of a target product is improved. A reaction process is simple. One-time investment of production devices and a production cost are reduced. Separation of a reaction product from the catalyst is simple. The method is prone to large-scale continuous industrial production.

Description

technical field [0001] The present invention relates to a method and device for preparing 1,2-propanediamine. Background technique [0002] 1,2-Propanediamine is an organic chemical intermediate and raw material with a wide range of uses. It is used in medicine, pesticide, organic synthesis, lubricating oil rust inhibitor, epoxy resin curing accelerator, spandex and modified shellac coatings There are important applications in the field, and its derivatives can also be used as rubber, coatings, raw materials, chelating agents and mineral processing agents, as well as the production of 1,2-propylene diamine tetraacetic acid as an intermediate of the anticancer drug propylene imine. [0003] The market demand for 1,2-propylene diamine is increasing year by year, and there are very few domestic products, mainly imported 1,2-propylene diamine to meet the market demand, which is mainly imported by BASF and other companies, which are expensive. At present, according to different ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/11C07C209/16B01J8/02
Inventor 严丽丁云杰吕元程显波马立新
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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