Catalyst used for synthesis of hexanediamine

A catalyst, a technology for hexamethylene diamine, which is applied in the field of catalysts for synthesizing hexamethylene diamine, can solve the problems of high toxicity of raw material adiponitrile, dependence on imports, hidden safety hazards, etc., so as to reduce one-time investment and production cost, and reduce operation difficulty. , the effect of improving safety

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 problems in the industrialized hydrogenation of adiponitrile to hexamethylenediamine: one is the Raney Ni catalyst commonly used in the route, which is easy to spontaneously ignite in the air, and there are major safety hazards in the preparation process; the other is The raw material adiponitrile is highly toxic, dependent on imports, expensive and subject to human

Method used

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  • Catalyst used for synthesis of hexanediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]5%Ni-15%Re-1.2%B / SiO 2 Catalyst preparation and application

[0027] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, and bake it at 500°C for 5 hours under an inert atmosphere. 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. The above SiO was impregnated with half of this aqueous solution 2 The carrier was air-dried, then dried at 120°C for 4 hours, and then calcined at 500°C for 4 hours. Then, the above SiO was impregnated for the second time with the remaining half of the aqueous solution 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 system is stable, the NH 3 / 1,6-Hexanediol = 5 (molar ratio) l...

Embodiment 2

[0029] 15%Ni-3.6%Re-1.2%B / SiO 2 Catalyst preparation and application

[0030] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, and bake it at 500°C for 5 hours under an inert atmosphere. 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

[0032] 30%Ni-0.2%Re-15%K / SiO 2 Catalyst preparation and application

[0033] Weigh 10 g carrier SiO 2 (20-40 mesh), the carrier SiO 2 Put it in a quartz tube, and bake it at 500°C for 5 hours under an inert atmosphere. 14.864 g Ni(NO 3 ) 2 6H2O, 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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Abstract

The invention relates to a catalyst used for synthesis of hexanediamine. The catalyst is composed of three parts, i.e., a main active component, an auxiliary agent and a carrier, wherein the main active component is Ni or Co; the auxiliary agent is one or more selected from the group consisting of metals or oxides like Fe, Cu, Ru, Re, K, Zn and B; the carrier is selected from SiO2 or Al2O3; the weight of the main active component accounts for 1 to 40% of the total weight of the catalyst; and the weight of the auxiliary agent accounts for 0.1 to 20% of the total weight of the catalyst. The catalyst provided by the invention undergoes an ammoniation reaction of hexanediol or aminohexanol or a hexanediol/aminohexanol mixture, so a hexanediamine product is synthesized under a hydrogen condition, and high activity, selectivity and stability are shown.

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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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889B01J23/755B01J23/75C07C209/16C07C211/12
CPCB01J23/889B01J23/75B01J23/755C07C209/16C07C211/12
Inventor 丁云杰严丽吕元
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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