Regeneration and Conversion of the Acetamide-Ammonium Acetate Catalytic System in the H2O2-Based Hydrazine Hydrate Production Process

doi:10.19894/j.issn.1000-0518.250119

Chinese Journal of Applied Chemistry ›› 2025, Vol. 42 ›› Issue (8): 1135-1143.DOI: 10.19894/j.issn.1000-0518.250119

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Regeneration and Conversion of the Acetamide-Ammonium Acetate Catalytic System in the H₂O₂-Based Hydrazine Hydrate Production Process

Guang-Hui JIAN¹, Fan YANG²(), Hong-Xin BAI², Yang WANG², Li-Ming JIA², Bao-Yi REN¹

^1.College of Science，Shenyang University of Chemical Technology，Shenyang 110000，China
^2.Sinopec （Dalian） Petrochemical Research Institute，Dalian 116000，China

Received:2025-03-20 Accepted:2025-06-23 Published:2025-08-01 Online:2025-08-11
Contact: Fan YANG
About author:yangfan.fshy@sinopec.com
Supported by:
the Joint Project of Science and Technology Planning of Liaoning Province(2024JH2/102600226)

Abstract

Abstract:

In order to study the recycle process of amide catalyst in the production of hydrazine hydrate by H₂O₂ method， the effects of reaction form， temperature， time， and ammonia flow rate process conditions on reaction equilibrium and acetamide yield were investigated for the dehydration of ammonium acetate to acetamide. The results showed that adopting a distillation reactor can significantly improve the reaction efficiency. The yield of acetamide can reach over 60% with a mass fraction （w） of no less than 80% after 3~4 h of reaction at 160 ℃， 300 mL/min ammonia flow rate. In addition， a continuous distillation experiment was conducted. The conditions were as follows： the introduction of the aqueous phase from methyl ethyl ketazine synthesis was into the reactor at a rate of 760.0 g/h， an ammonia flow rate was 650 mL/min， and a reflux ratio was 0.1. After the system stabilizes， the temperature of head was 93 ℃， and 554.4 g/h of distillate were collected overhead； The temperature of the boiler was 168 ℃， and 248.7 g/h of recycled catalyst were obtained by draining the boiler which the mass fraction of acetamide is 83.61%.

Key words: H₂O₂ method, Hydrazine hydrate, Recycle of catalyst, Dehydration of ammonium acetate, Acetamide, Reactive distillation

CLC Number:

O621.2

Guang-Hui JIAN, Fan YANG, Hong-Xin BAI, Yang WANG, Li-Ming JIA, Bao-Yi REN. Regeneration and Conversion of the Acetamide-Ammonium Acetate Catalytic System in the H₂O₂-Based Hydrazine Hydrate Production Process[J]. Chinese Journal of Applied Chemistry, 2025, 42(8): 1135-1143.

Figures/Tables 8

Fig.1 Mass fraction and yield of acetamide with autoclave at different temperatures

Fig.2 The relationship of acetamide mass fraction （A） and yield （B） against reaction time at different temperatures with autoclave

Fig.3 Acetamide mass fraction after 6 h reaction in autoclave and distillation reactor at different temperatures

Fig.4 The relationship between acetamide mass fraction （A） and yield （B） against reaction time at different temperatures with distillation reactor

Fig.5 The loss rate of ammonium acetate and the thermal decomposition rate of the substance after 6 h reaction at different temperatures with distillation reactor

Fig.6 The relationship of acetamide mass fraction （A） and yield （B） against against reaction time with different ammonia flow rate

Fig.7 The loss rate of ammonium acetate and the thermal decomposition rate of substance after 6 h reaction at different ammonia flow rates with distillation reactor

Table 1 Composition mass of introduction and discharge in continuous distillation experiment

w（composition）/%	Feedstock/%	Bottom product/%	Overhead product/%
CH₃CONH₂	18.01	83.61	0
CH₃COONH₄	20.09	1.22	0
MEK	1.52	0	2.08
KET	0.78	0	1.06
H₂O₂	53.39	0	83.70
NH₃	6.21	0	13.16
CH₃COOH	0	15.17	0

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Regeneration and Conversion of the Acetamide-Ammonium Acetate Catalytic System in the H₂O₂-Based Hydrazine Hydrate Production Process

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