Catalyst for synthesizing hexamethylenediamine

A catalyst, the technology of hexamethylenediamine, which is applied in the field of catalysts for the synthesis of hexamethylenediamine, can solve the problems of unfavorable large-scale continuous industrial production, poor selectivity, and harsh reaction conditions, so as to reduce one-time investment and production costs and improve selectivity and stability, optimize the effect of reaction conditions

Inactive Publication Date: 2017-06-09
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

Judging from the current existing literature and technologies, most of the production technologies of hexamethylenediamine have disadvantages such as poor selectivity, difficult product separation, harsh reaction conditions, and low yield. The preparation methods are not conducive to large-scale continuous industrial production.
There are still two fatal...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 5%Ni-15%Re-1.2%B / SiO 2 Catalyst preparation and application

[0028] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 10% ammonia-hydrogen gas mixture, the ammoniation temperature is 300°C, and the ammoniation time is 5 hours. 2.477 g Ni(NO 3 ) 2 ·6H 2 O, 2.161 g NH 4 ReO 4 and 0.686 g H 3 BO 3 Dissolve in 12ml deionized water. Half of this aqueous solution was used to impregnate the above ammoniated SiO 2 The carrier was air-dried, then dried at 120°C for 4 hours, and then calcined at 500°C for 4 hours. Then, impregnate the ammonified SiO 2 The carrier is then air-dried, dried at 120°C for 4 hours, and calcined at 500°C for 4 hours. Before the catalyst is used, in a hydrogen flow at 375°C (atmospheric pressure, 2000h -1 ) to reduce for 4 hours. When the temperature in the reactor is naturally lowered to 160°C, the pressure is increased to 8MPa. After the s...

Embodiment 2

[0030] 15%Ni-3.6%Re-1.2%B / SiO 2 Catalyst preparation and application

[0031] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 20% ammonia-hydrogen gas mixture, the ammoniation temperature is 300°C, and the ammoniation time is 5 hours. 7.432 g Ni(NO 3 ) 2 ·6H 2 O, 0.518 g NH 4 ReO 4 and 0.686 g H 3 BO 3 Dissolve in 12ml deionized water. Refer to Example 1 for the remaining preparation steps and catalyst evaluation scheme. The reaction results are shown in Table 1.

Embodiment 3

[0033] 30%Ni-0.2%Re-15%K / SiO 2 Catalyst preparation and application

[0034] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, dry at 200°C for 5 hours under an inert atmosphere, then introduce 50% ammonia-hydrogen gas mixture, the ammoniation temperature is 300°C, and the ammoniation time is 5 hours. 14.864 g Ni(NO 3 ) 2 ·6H 2 O, 0.029 g NH 4 ReO 4 and 3.879 grams of KNO 3 Dissolve in 12ml deionized water. Refer to Example 1 for the remaining preparation steps and catalyst evaluation scheme. The reaction results are shown in Table 1.

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PUM

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Abstract

The invention relates to a catalyst for synthesizing hexamethylenediamine. The catalyst is composed of three parts, namely a main active ingredient, aids and a carrier subjected to ammoniated treatment, wherein the main active ingredient is Ni or Co; the aids refer to one or more ofmetals such as Fe, Cu, Ru, Re, K, Zn and B or oxides; and the carrier subjected to ammoniated treatment is selected from SiO2 or Al2O3 subjected to ammoniated treatment. In the total weight of the catalyst, the main active ingredient accounts for 1-40%, and the aids account for 0.1-20%. The catalyst disclosed by the invention has the characteristic that the adopted carrier needs special ammoniated treatment. According to the catalyst disclosed by the invention, an ammonolysis reaction of hexanediol or amino hexanol or a hexanediol/amino hexanol mixture is implemented, the hexamethylenediamine product is synthesized under a hydrogen present condition, and the catalyst has high activity, high selectivity and stability.

Description

technical field [0001] The invention relates to a catalyst for synthesizing hexamethylenediamine and its application. In more detail, it relates to a catalyst for converting hexanediol or aminohexanol or a mixture of hexanediol / aminohexanol and ammonia into hexamethylenediamine under the condition of hydrogen. Background technique [0002] Hexamethylenediamine is an important organic chemical intermediate, mainly used in the production of polyamides, such as nylon 66 salt, nylon 610, nylon 612 and nylon 69; it can also be used to synthesize diisocyanate or epoxy resin and urea Resin curing agent, organic crosslinking agent, etc. With the continuous development of the synthetic fiber industry, the demand for hexamethylenediamine compounds worldwide continues to increase, the price continues to rise, and the gap between market supply and demand is relatively large. [0003] The production processes of hexamethylenediamine mainly include caprolactam method, butadiene method, ...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J23/78B01J23/889B01J27/24C07C209/16C07C211/12C07C213/02C07C215/08C07D295/027C07D295/023
CPCB01J23/8896B01J23/755B01J23/78B01J27/24C07C209/16C07C213/02C07D295/023C07D295/027C07C211/12C07C215/08
Inventor 严丽丁云杰吕元
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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