骨架镍的制备及其在染料中间体合成中的应用

doi:10.13475/j.fzxb.20190802407

纺织学报 ›› 2020, Vol. 41 ›› Issue (11): 95-101.doi: 10.13475/j.fzxb.20190802407

骨架镍的制备及其在染料中间体合成中的应用

冯鹏耀¹, 王蓉¹, 瞿建刚¹^,², 董玲¹, 胡啸林¹^,²()

1.南通大学纺织服装学院, 江苏南通 226019
2.东华大学纺织面料技术教育部重点实验室, 上海 201620

收稿日期:2019-08-09 修回日期:2020-08-07 出版日期:2020-11-15 发布日期:2020-11-26
通讯作者: 胡啸林
作者简介:冯鹏耀(1995—),男,硕士生。主要研究方向为纺织印染助剂及新技术研发。
基金资助:
南通市基础科学研究项目(JC2018036);南通大学纺织服装学院研究生自主创新项目(FZ201814)

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. 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

摘要/Abstract

摘要：

为满足清洁生产的要求,提高T酸合成的反应速率和转化率,以镍铝合金粉末作为催化剂前驱体,经过氢氧化钠活化制备骨架镍催化剂,借助扫描电子显微镜、X射线衍射仪、比表面积及孔隙分析仪和Zeta电位分析仪等手段对其结构和性能进行表征,并研究其在硝基T酸加氢还原制备T酸中的应用。结果表明:制备的骨架镍催化剂含有大量的孔道,以中孔为主,比表面积为46.88 m²/g,平均晶粒尺寸为15.8 nm。制备的骨架镍在硝基T酸加氢还原中的最佳应用工艺为:催化剂质量分数2.500%,反应压力2.0 MPa,反应温度120 ℃,搅拌速度800 r/min。在此最佳工艺条件下,硝基T酸的转化率达99.07%,并且套用10次无明显失活现象。

关键词: 骨架镍, 硝基T酸, 催化加氢, T酸, 染料中间体

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

中图分类号:

TQ612.3

冯鹏耀, 王蓉, 瞿建刚, 董玲, 胡啸林. 骨架镍的制备及其在染料中间体合成中的应用[J]. 纺织学报, 2020, 41(11): 95-101.

FENG Pengyao, WANG Rong, QU Jian'gang, DONG Ling, HU Xiaolin. Preparation of Raney nickel and its application in synthesis of dye intermediates[J]. Journal of Textile Research, 2020, 41(11): 95-101.

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元素种类	质量分数/%
元素种类	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

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

骨架镍的制备及其在染料中间体合成中的应用

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

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