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Catalyst used for catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol as well as preparation and application of catalyst

A technique for synthesizing fatty alcohols and catalyzing primary amines, which is used in the field of catalyzing the synthesis of fatty tertiary amines from primary or secondary amines and fatty alcohols. It can solve the problem of declining economic benefits of alkyl fatty tertiary amines and raising industrial production costs by precious and rare metal elements. and other problems, to achieve the effect of easy-to-obtain raw materials, low cost, easy operation, and no need for solvents

Active Publication Date: 2017-03-22
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the utilization of precious and rare metal elements will greatly increase the cost of industrial production, resulting in a significant decline in the economic benefits of producing alkyl fatty tertiary amines

Method used

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  • Catalyst used for catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol as well as preparation and application of catalyst
  • Catalyst used for catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol as well as preparation and application of catalyst
  • Catalyst used for catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol as well as preparation and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Catalyst preparation:

[0034] Mix and dissolve a calculated amount of required metal nitrate solid and a certain amount of deionized water in a beaker, heat to 323K and magnetically stir to dissolve completely. Co-precipitation method is adopted in the process of preparing the catalyst, and the precipitation agent is NaOH+Na 2 CO 3, the molar ratio is 1:1, and the mass fraction is about 10%. First, the precipitant is evenly pumped into the beaker containing the aluminum nitrate solution by a peristaltic pump at an initial flow rate of 5 mL / min, the magnetic stirring speed is 5 r / s, and the temperature in the beaker is raised to 353 K, so that the aluminum nitrate solution is finally completely converted into Aluminum hydroxide gel, and then add the nitrate solution of the active components in the order of Ni, Mg, Cu, Fe for co-precipitation, and maintain the pH value of the solution at about 9 by adjusting the flow rate pumped by the peristaltic pump. After the drop...

Embodiment 2

[0038] Alkylation of primary amines

[0039]

[0040] Add n-propylamine (0.15mol) and n-octanol (0.6mol) to a 300mL three-necked flask in sequence, add 0.02mol catalyst, feed hydrogen at a flow rate of 0.2L / min, and heat to 190°C for 7h. Samples were taken every hour, and the product was separated and purified by column chromatography. GC-MS detected that the yield of aliphatic tertiary amine increased with the increase of reaction time, reaching a maximum of 96.35% at the 6th hour, and the conversion rate and selectivity were 97.56% respectively. and 98.75%, and then the yield remained stable. The catalyst prepared by Example 1, the components and proportioning ratio are: Ni:Cu:Mg:Fe=1.25:1:0.3:0.6, and its mass fractions are respectively: nickel: 21.75%; copper: 18.95%; magnesium: 4.25% %; Iron: 6.32%.

[0041] After the reaction, filter, wash and dry to obtain the reacted catalyst. After using this catalyst to participate in the reaction repeatedly for 4 times, it can...

Embodiment 3

[0043] Alkylation of secondary amines

[0044]

[0045] Add di(n-propyl)amine (0.15mol) and n-octanol (0.3mmol) successively into a 300mL three-necked flask, add 0.02mol of catalyst, feed hydrogen at a flow rate of 0.2L / min, and heat to 190°C for 7h. Samples were taken every hour, and the product was separated and purified by column chromatography. GC-MS detected that the yield of aliphatic tertiary amine increased with the increase of reaction time, reaching a maximum of 97.33% at the 6th hour, and the conversion rate and selectivity were 98.56% respectively. and 98.75%, and then the yield remained stable. The catalyst prepared by Example 1, the components and the proportioning ratio are: Ni:Cu:Mg:Fe=1.25:1:0.3:0.6, and its mass fractions are respectively: nickel: 21.75%; copper: 18.95%; magnesium: 4.25% %; Iron: 6.32%.

[0046] After the reaction, filter, wash and dry to obtain the reacted catalyst. After using the catalyst to repeatedly participate in the reaction for...

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Abstract

The invention discloses a catalyst used for catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol as well as a preparation and an application of the catalyst. The catalyst comprises catalytic activity components including nickel, copper, magnesium and iron and an active aluminum oxide carrier; the preparation method of the catalyst is implemented as follows: nitrates of Ni, Mg, Cu and Fe are taken as catalytic activity component raw materials, aluminum hydroxide gel is taken as a carrier raw material, NaOH and Na2CO3 are taken as precipitators, and a catalyst precursor is obtained with a coprecipitation method; the catalyst precursor is roasted and then reduced and activated by KBH4, and the catalyst is obtained; the catalyst has the characteristics of high selectivity and high conversion rate when catalyzing synthesis of aliphatic tertiary amine from primary amine or secondary amine and fatty alcohol, the reaction process is simple, the reaction time is short, requirements for equipment are low, raw materials are easy to obtain, the cost is low, and no solvent is required.

Description

technical field [0001] The invention relates to a catalyst for catalyzing the synthesis of fatty tertiary amines from primary or secondary amines and fatty alcohols, in particular to a catalytically active component containing nickel, copper, magnesium and iron supported on an active aluminum oxide carrier The catalyst constituted above, as well as the preparation method of the catalyst and its application in catalyzing the synthesis of fatty tertiary amines from primary or secondary amines and fatty alcohols belong to the field of chemical synthesis. Background technique [0002] With single long chain alkyl tertiary amine, double long chain alkyl tertiary amine and three long chain alkyl tertiary amine (respectively RNMe 2 , R 2 NMe and R 3 N) Alkyl tertiary amines with three structures are widely used as a class of important organic intermediates in cationic surfactants, amphoteric compounds, dye auxiliaries and fungicides, etc. Trialkyl tertiary amines are alkyl fats ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78C07C209/16C07C211/08
CPCB01J23/78C07C209/16C07C211/08
Inventor 周涛潘明希邱天韵
Owner CENT SOUTH UNIV
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