Modification method for raney nickel catalyst for p-chloronitrobenzene hydrogenation
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of p-nitrochlorobenzene and skeleton nickel, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problem that skeleton nickel catalysts cannot be more widely used , less research on the modification of framework nickel catalysts, etc., to achieve the effect of reducing subsequent treatment processes and reducing costs
Inactive Publication Date: 2012-07-04
CHINA PETROLEUM & CHEM CORP +1
View PDF6 Cites 4 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
However, there are few studies on the modification of later-stage framework nickel catalysts.
However, the requirements for framework nickel catalysts in organic chemical hydrogenation processes are different, which prevents framework nickel catalysts from being more widely used in various hydrogenation processes.
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0014] Get unmodified skeleton nickel catalyst 10g, add deionized water 30g, Zn(NO 3 ) 2 3g. Add it to a 100ml beaker at 50°C for 30 minutes with magnetic stirring, let it stand for 60 minutes, add 60 g of hypophosphorous acid solution as a reducing agent, stir it with magnetic force for 45 minutes, and use NaHCO 3 Adjust the pH value to 9. Let it stand for 45 minutes, wash with water until neutral, and filter to obtain a modified skeleton nickel catalyst.
[0015] Evaluation of p-chloronitrobenzene hydrogenation: the conversion rate of p-chloronitrobenzene is 96%, the selectivity is ≥94%, and the yield is ≥92%.
Embodiment 2
[0017] Take 10g of unmodified skeleton nickel catalyst, add 30g of deionized water, CuSO 4 3g. Add it to a 100ml beaker at 50°C for 30 minutes with magnetic stirring, let it stand for 60 minutes, add 60 g of hypophosphorous acid solution as a reducing agent, stir it with magnetic force for 45 minutes, and use NaHCO 3 Adjust the pH value to 9. Let it stand for 45 minutes, wash with water until neutral, and filter to obtain a modified skeleton nickel catalyst.
[0018] Evaluation of p-chloronitrobenzene hydrogenation: the conversion rate of p-chloronitrobenzene is 98%, the selectivity is ≥95%, and the yield is ≥93%.
Embodiment 3
[0020] Get unmodified skeleton nickel catalyst 10g, add deionized water 30g, Cr(NO 3 ) 3 3g. Add it to a 100ml beaker at 50°C for 30 minutes with magnetic stirring, let it stand for 60 minutes, add 60 g of hypophosphorous acid solution as a reducing agent, stir it with magnetic force for 45 minutes, and use NaHCO 3 Adjust the pH value to 9. Let it stand for 45 minutes, wash with water until neutral, and filter to obtain a modified skeleton nickel catalyst.
[0021] Evaluation of p-chloronitrobenzene hydrogenation: the conversion rate of p-chloronitrobenzene is 98%, the selectivity is ≥93%, and the yield is ≥90%.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Login to view more
Abstract
The invention relates to a modification method for a raney nickel catalyst for p-chloronitrobenzene hydrogenation, and belongs to the technical field of organic synthesis. According to the method, a catalyst is added to deionized water containing 1-5% of a modifier, a stirring reaction is performed for 20-40 minutes at a temperature of 30-70 DEG C, and a standing treatment is performed for 30-90 minutes; a reduction agent with the concentration of 5-15% is added, a stirring reaction is performed for 30-60 minutes at the temperature of 40-50 DEG C, and NaHCO3 is adopted to adjust the pH value to 8-10, wherein a mass ratio of the reduction agent to the raney nickel catalyst is 4:1-8:1; a standing treatment is performed for 30-60 minutes, and deionized water is adopted to wash until the solution is neutral, a filtering treatment is performed, water is added, and sealed preservation is performed to prepare the modified raney nickel catalyst. According to the present invention, under the condition of no addition of the dechlorination inhibitor, the p-chloronitrobenzene conversion rate is more than or equal to 99.9%, the dechlorination side reaction generation rate in the p-chloronitrobenzene hydrogenation process is less than or equal to 2%, and the yield of p-chloroaniline is more than or equal to 95%; compared to the existing methods for preparing the hydrogenation catalyst, the method of the present invention has the following advantages that: the hydrogenation process is simplified, the three waste is less after the hydrogenation, the cost is low, the energy consumption is low, and the industrial requirements of quality increasing, consumption reducing, and environmental protection are achieved.
Description
technical field [0001] The invention belongs to the technical field of organic synthesis, and proposes a method for modifying and modifying a skeleton nickel catalyst for hydrogenation of p-chloronitrobenzene. Background technique [0002] Nickel (Raney Ni) is an extremely important catalyst for hydrogenation. It has been widely used in the hydrogenation process, such as the hydrogenation of alkynes, alkenes, aryls, carbonyls, nitro groups and nitrile groups. The quantity is also larger. The catalytic reaction process of nickel catalyst is roughly divided into four steps: (1) hydrogen adsorption on the surface of nickel metal particles and split into hydrogen atoms; (2) adsorption of reactants; (3) surface reaction; (4) product desorption. Therefore, in the hydrogenation process, the activity and service life of the Raney nickel catalyst directly affect the quality, yield and economic benefits of the product. With the improvement of catalyst performance requirements in the...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to view more 
Login to view more