Supported Ni-Cu-Cr catalyst and application thereof

A ni-cu-cr, catalyst technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problems of low polyether amination rate, etc. High ether amination rate, low polyether amination rate and good practicability

Inactive Publication Date: 2015-04-01
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Purpose of the invention: In view of the deficiencies in the prior art, the purpose of the present invention is to provide a supported Ni-Cu-Cr catal

Method used

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  • Supported Ni-Cu-Cr catalyst and application thereof
  • Supported Ni-Cu-Cr catalyst and application thereof
  • Supported Ni-Cu-Cr catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0038] Example 1

[0039] Weigh the nitrate corresponding to the metal salt (Ni(NO 3 ) 2 , Cu(NO 3 ) 2 , Cr(NO 3 ) 2 ), prepare a 1mol / L mixed solution with deionized water, where n(Ni):n(Cu):n(Cr)=20:5:1; in the same way, configure a 1mol / L alkaline solution as a precipitation agent. Under strong stirring at 60℃, add the metal salt solution dropwise to Na 2 CO 3 In the solution, the catalyst precursor was obtained by aging, washing, suction filtration, and drying in an oven at 105°C for 10 hours. The obtained precursor is uniformly mixed with the carrier M, and the carrier content is controlled to 20%, and then transferred to the muffle furnace through milling and granulation, and calcined with a programmed temperature (10℃ / min) to 330℃ for 2h, and then the calcined catalyst Press the tablet, and finally transfer to the reduction activation device, in the H 2 Under the environment (180℃ reduction 2h, 400℃ reduction 8h, H 2 The flow rate is 80mL / min) for the reduction and activat...

Example Embodiment

[0048] Example 2

[0049] Preparation of Ni-Cu-Cr catalyst: Weigh the nitrate corresponding to the metal salt (Ni(NO 3 ) 2 , Cu(NO 3 ) 2 , Cr(NO 3 ) 2 ), prepare a 1mol / L mixed solution with deionized water, where n(Ni):n(Cu):n(Cr)=20:5:1; in the same way, configure a 1mol / L alkaline solution as a precipitation agent. Under strong stirring at 60℃, add the metal salt solution dropwise to Na 2 CO 3 In the solution, the catalyst precursor was obtained by aging, washing, suction filtration, and drying in an oven at 105°C for 10 hours. Prepare precursor and carrier γ-Al 2 O 3 Mix uniformly, control the amount of added carrier to be 5%, 10%, 15%, 20% respectively, then transfer to the muffle furnace through milling and granulation, and use the programmed temperature (10°C / min) to roast at 350°C for 2h, and then The calcined catalyst is pressed into tablets, and finally transferred to the reduction activation device. 2 Under the environment (180℃ reduction 2h, 400℃ reduction 8h, H 2 The...

Example Embodiment

[0052] Example 3

[0053] The preparation of the Ni-Cu-Cr catalyst is the same as in Example 2. The Ni-Cu-Cr catalyst has no support added, and Ni-Cu-Cr / Al 2 O 3 When blended γ-Al 2 O 3 The amount of carrier is 10%.

[0054] The performance evaluation of the hydroamination reaction is the same as in Example 1.

[0055] Recycling of the catalyst: the catalyst filtered out in the subsequent treatment of the hydroamination reaction is washed three times with 100 mL ethanol, dried in an oven at 105°C for 10 hours, and then used in the next hydroamination reaction.

[0056] The recycling effect of the catalyst is shown in Table 2. In multiple uses, the catalyst performance after adding the support is better than the sample without adding the support.

[0057] Table 2 Comparative experiments and recycling of catalysts

[0058]

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Abstract

The invention discloses a supported Ni-Cu-Cr catalyst and application thereof. The supported Ni-Cu-Cr catalyst is prepared by adopting a method which comprises the following steps: preparing an Ni-Cu-Cr precursor by adopting a coprecipitation method; (2) blending with a carrier for granulation; (3) tabletting a calcined catalyst, and reducing at 180 DEG C for 2 hours and reducing at 400 DEG C for 8 hours in an H2 environment, wherein the flow velocity of H2 is 60-100mL/min. The supported Ni-Cu-Cr catalyst disclosed by the invention can be used for effectively solving the problem of low amination rate of polyether, innovating the condition of a process for synthesizing end-amino polyether by adopting a direct amination catalysis method, and achieving that the amination rate is 50%-55% and the selectivity of primary amine is up to 95%-98% in a prescribed autoclave process and a prescribed tubular reactor process, has very good practicability and can achieve very good economic benefits and social effects.

Description

technical field [0001] The invention relates to the technical field of catalysts for organic compound synthesis, in particular to a supported Ni-Cu-Cr catalyst and its application. Background technique [0002] Amine Terminated Polyether (ATPE for short) is a kind of polyalkylene oxide compound terminated by primary or secondary amino groups, which can be divided into various series of products according to molecular weight and number of functional groups. The specific molecular structure determines its unique properties and special applications. They are widely used in polyurethane / polyurea, epoxy resin curing agent, surfactant and other fields. [0003] The only difference between amino-terminated polyether and ordinary polyether is that the hydroxyl groups at the chain ends are replaced by amino groups. However, it is precisely because of the change of the terminal functional group that the reactivity of the amino-terminated polyether has been greatly improved, especiall...

Claims

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Application Information

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IPC IPC(8): B01J23/86C07C217/08C07C213/02
Inventor 朱新宝陈慕华吴永忠吕耀武
Owner NANJING FORESTRY UNIV
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