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Method and device for preparing propane diamine by taking propylene glycol and liquid ammonia as raw materials

A technology of propylene glycol and propylenediamine, which is applied in the field of preparation of propylenediamine, can solve the problems of harsh reaction conditions, low selectivity of propylenediamine, unfavorable preparation methods for large-scale continuous industrial production, etc., to achieve high selectivity and improve selectivity Sexuality, the effect of reducing one-time investment and production cost

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 existing at present are that the conditions of the reaction are harsh, the selectivity of propylenediamine is relatively low, and the preparation method is not conducive to large-scale continuous industrial production

Method used

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  • Method and device for preparing propane diamine by taking propylene glycol and liquid ammonia as raw materials
  • Method and device for preparing propane diamine by taking propylene glycol and liquid ammonia as raw materials
  • Method and device for preparing propane diamine by taking propylene glycol and liquid ammonia as raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Weigh the above 15%Ni-1.6%Re-1.2%B / Al 2 o 3 Catalyst 3.2 grams (about 4ml), is packed in the fixed-bed reactor. The catalyst is activated by hydrogenation treatment before use. The activation conditions are: temperature T=375°C; pressure P=atmospheric pressure, gas volume space velocity GHSV=2000h -1 , the reduction time is 4 hours. When the temperature in the reactor is naturally lowered to 140°C, the pressure is increased to 8MPa. After the system is stable, the liquid ammonia / 1,2-propylene glycol=10 (molar ratio) is pumped into the reactor to adjust the liquid of propylene glycol. The volume space velocity is 0.5h -1 , H in the reaction system 2 The content was 2.5 mol%, and the reaction was carried out, and the reaction time was 50 hours, and a sample was taken for analysis. SE-30 capillary column, FID detector, N,N-dimethylformamide as internal standard for quantitative analysis, the reaction results are shown in Table 1. The product is distilled under reduce...

Embodiment 2

[0051] Weigh the above 15%Ni-1.6%Re-1.2%B / Al 2 o 3 Catalyst 3.2 grams (about 4ml), is packed in the fixed-bed reactor. The catalyst is activated by hydrogenation treatment before use. The activation conditions are: T=375°C; P=atmospheric pressure, GHSV=2000h -1 , the reduction time is 4 hours. When the temperature in the reactor is naturally lowered to 160°C, the pressure is raised to 8MPa. After the system is stable, the liquid ammonia / 1,2-propanediol=10 (molar ratio) is pumped into the reactor to adjust the liquid of propylene glycol. The volume space velocity is 0.5h -1 , H in the reaction system 2 The content was 2.5 mol%, and the reaction was carried out, and the reaction time was 50 hours, and a sample was taken for analysis. SE-30 capillary 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 Catalyst 3.2 grams (about 4ml), is packed in the fixed-bed reactor. The catalyst is activated by hydrogenation treatment before use. The activation conditions are: T=375°C; P=atmospheric pressure, GHSV=2000h -1 , the reduction time is 4 hours. When the temperature in the reactor is naturally lowered to 170°C, the pressure is increased to 8MPa. After the system is stable, the liquid ammonia / 1,2-propanediol=10 (molar ratio) is pumped into the reactor to adjust the liquid of propylene glycol. The volume space velocity is 0.5h -1 , H in the reaction system 2 The content was 2.5 mol%, and the reaction was carried out, and the reaction time was 50 hours, and a sample was taken for analysis. SE-30 capillary 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 for preparing propane diamine by taking propylene glycol and liquid ammonia as raw materials. Propylene glycol and liquid ammonia are mixed in a certain ratio and are pumped into a reactor by virtue of a pump, and reaction is carried out in presence of a catalyst and hydrogen. The method for preparing the propane diamine by taking the propylene glycol and liquid ammonia as the raw materials has the advantages that a novel catalyst is adopted, catalytic performance is excellent, and long-time operation can be easily carried out; propylene glycol is subjected to hydroamination for producing a propane diamine product at lower reaction pressure, and reaction conditions are adjusted and changed, so that composition of the product can be flexibly adjusted and changed, selectivity of a target product is improved, a reaction process is simple, one-time investment of a production unit and production cost are reduced, a reaction product and a catalyst can be simply separated, and large-scale continuous industrial production can be easily realized.

Description

technical field [0001] The invention relates to a method and a device for preparing propylenediamine. Background technique [0002] Propylenediamine includes 1,2-propylenediamine and 1,3-propylenediamine. 1,2-Propylenediamine is an organic chemical intermediate and raw material with a wide range of uses. It has important applications in the field, and its derivatives can also be used as rubber, coatings, raw materials, chelating agents, mineral processing agents, etc., and the production of 1,2-propylenediaminetetraacetic acid as an intermediate for anticancer drug propyleneimine. 1,3-Propylenediamine is a low-grade aliphatic diamine with active chemical properties. It can be widely used in pharmaceutical, pesticide, dye, petrochemical, semiconductor manufacturing and polymer industries. It is an important fine organic chemical intermediate. With the development of society and science and technology, the application range of 1,2-propanediamine and 1,3-propanediamine is con...

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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