Journal of Textile Research ›› 2020, Vol. 41 ›› Issue (11): 95-101.doi: 10.13475/j.fzxb.20190802407

• Dyeing and Finishing & Chemicals • Previous Articles     Next Articles

Preparation of Raney nickel and its application in synthesis of dye intermediates

FENG Pengyao1, WANG Rong1, QU Jian'gang1,2, DONG Ling1, HU Xiaolin1,2()   

  1. 1. College of Textile and Clothing, Nantong University, Nantong, Jiangsu 226019, China
    2. Key Laboratory of Textile Science & Technology, Ministry of Education, Donghua University, Shanghai 201620, China
  • Received:2019-08-09 Revised:2020-08-07 Online:2020-11-15 Published:2020-11-26
  • Contact: HU Xiaolin E-mail:nthxl2006@126.com

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Abstract:

In order to meet the requirements for clean production and to improve the reaction rate and conversion rate of T-acid synthesis, the nickel-aluminum alloy powder was used as the catalyst precursor to prepare the Raney nickel catalyst by sodium hydroxide activation. The prepared structure and properties of the materials were studied by means of scanning electron microscope, X-ray diffractometer, specific surface area and pore structure tester and Zeta potential tester, and so on, and its application in the preparation of T-acid by hydrogenation reduction of nitro T-acid was investigated. The results show that the prepared Raney nickel catalyst is rich in pore structures, mainly mesopores, with a specific surface area of 46.88 m2/g and an average grain size of 15.8 nm. The optimum application process of the prepared Raney nickel in the hydrogenation reduction of nitro T-acid is as follows: catalyst dosage 2.500%, reaction pressure 2.0 MPa, reaction temperature 120 ℃, stirring speed 800 r/min. Under the best process conditions, the conversion of nitro T-acid reaches 99.07%, and there is no obvious deactivation after ten times of reuse.

Key words: Raney nickel, nitro T-acid, catalytic hydrogenation, T-acid, dye intermediate

CLC Number: 

  • TQ612.3

Fig.1

Nitro T-acid hydrogenation reaction equation"

Fig.2

XRD pattern of aluminum-nickel alloy"

Fig.3

XRD pattern of raney nickel"

Fig.4

SEM images of aluminum-nickel alloy (a) and Raney nickel(b) "

Tab.1

Main component content of aluminum-nickel alloy and Raney nickel"

元素种类 质量分数/%
镍铝合金 骨架镍
Ni 59.3 54.4
Al 36.7 14.4
C 4.0 4.3
O 0 26.9

Fig.5

N2 adsorption-desorption isotherms of Raney nickel and aluminum-nickel alloy"

Fig.6

Pore size distribution curves of Raney nickel"

Tab.2

Specific surface area and pore structure parameters of Raney nickel"

比表面积SBET/
(m2·g-1)		 总孔容VP/
(cm3·g-1)		 平均孔径D/
nm		 DFT全孔径分析
微孔率/
%		 中孔率/
%		 大孔率/
%
46.88 0.063 5.4 0 95.20 4.80

Fig.7

Zeta potential of aluminum-nickel alloy and Raney nickel"

Fig.8

Nitro T-acid hydrogenation reduction process. (a)Amount of catalyst;(b)Reaction pressure;(c)Reaction temperature;(d)Stirring speed"

Fig.9

Reuse experiment result"

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