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Catalyst for reaction for producing diethylenetriamine by means of hydrogenation of ethylenediamine, and preparation method of catalyst

A technology for preparing diethylenetriamine and catalyst, which can be applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, preparation of amino compounds by disproportionation, etc. Problems such as poor sexuality, to achieve the effect of obvious advantages

Active Publication Date: 2018-11-09
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a high activity and high selectivity catalyst for diethylenetriamine hydrogenation of ethylenediamine and its Preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.1g of palladium acetate and 3.74g of lanthanum nitrate hexahydrate into a mixed solution of 30mL of water and 30mL of ethanol and fully shake to obtain solution A. Under the condition of 10KPa, add solution A dropwise into a rotary evaporator equipped with 40gФ2mm diameter γ-shaped alumina balls, and rotate at a speed of 30r / min, gradually heat to 60°C, wait until the solvent is completely evaporated, take out And dry at 80°C to obtain solid particles B; then dissolve 19.82g nickel nitrate hexahydrate, 19.98g cobalt nitrate hexahydrate and 6.6g copper nitrate in 30mL water and 30mL ethanol to obtain solution C, and then dissolve the obtained solution C Add dropwise into the rotary evaporator equipped with solid particles B, rotate at a speed of 30r / min and gradually heat until the solvent is evaporated completely, take it out, dry at 80°C, and roast at 500°C for 6h, that is Catalyst I was obtained.

Embodiment 2

[0022] Add 0.05g of palladium nitrate and 1.8g of cerium acetate into a mixed solution of 20mL of water and 10mL of ethanol, and shake fully to obtain solution D. Under the condition of 10KPa, add solution D dropwise to the rotary evaporator equipped with 20gФ3mm diameter θ-type alumina balls, and rotate at a speed of 30r / min, gradually heat to 60°C, wait until the solvent is completely evaporated, take out And dry at 80°C to obtain solid particles E; then dissolve 19.82g of nickel acetate tetrahydrate, 19.98g of cobalt nitrate hexahydrate and 6.6g of copper acetate in 30mL of water and 30mL of ethanol to obtain solution F, and then dissolve the resulting solution F Add it dropwise into the rotary evaporator equipped with solid particles E, rotate at a speed of 30r / min and gradually heat until the solvent is completely evaporated, take it out, dry it at 80°C, and roast it at 450°C for 6h, that is Catalyst II was obtained.

Embodiment 3

[0024] Add 0.1g of palladium acetate and 4.06g of lanthanum nitrate hexahydrate into a mixed solution of 30mL of water and 30mL of ethanol, and fully shake to obtain solution G. Under the condition of 10KPa, add solution G dropwise to the rotary evaporator equipped with 40g 3mm long γ-shaped aluminum oxide strips, and rotate at a speed of 30r / min, gradually heat to 60°C, and wait for the solvent to evaporate completely , taken out and dried at 80°C to obtain solid particles H; then 19.98g of cobalt nitrate hexahydrate and 6.6g of copper acetate were dissolved in 30mL of water and 30mL of ethanol to obtain solution I, and then the obtained solution I was added dropwise to the container In a rotary evaporator with solid particles H, rotate at a speed of 30r / min and gradually heat until the solvent is completely evaporated, take it out, dry it at 80°C, and calcinate it at 400°C for 8 hours to obtain catalyst III.

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Abstract

The invention relates to a catalyst for a reaction for producing diethylenetriamine by means of hydrogenation of ethylenediamine, and a preparation method of the catalyst, aiming at solving the problems that the existing catalyst is low in activity and selectivity. The catalyst takes alumina as a carrier, and contains 0.1-3wt% of one or two or more of rare earth elements, 5-30wt% of one or two ormore of nickel, copper, iron, cobalt, zinc or tin, and 0.1-5wt% of palladium based on the total weight of the catalyst. The catalyst is prepared by firstly coating the carrier with the palladium element and the rare earth elements, and then coating the carrier with the other elements. The catalyst provided by the invention is used for catalyzing the reaction for producing the diethylenetriamine bymeans of the hydrogenation of the ethylenediamine, can obviously improve reaction activity and product selectivity, and has a very high industrial application value.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a catalyst for hydrogenating ethylenediamine to diethylenetriamine and a preparation method thereof. Background technique [0002] Diethylenetriamine is an important organic synthesis intermediate, widely used in epoxy resin curing agent, crude oil demulsifier, mining additives, lubricating oil additive, surfactant, paper strengthening agent, polyamide resin, metal chelate Mixture, cyanide-free electroplating additives and other fields. [0003] In the prior art, the hydrogenation catalytic synthesis of diethylenetriamine using ethylenediamine as a raw material has attracted more and more attention due to its advantages of less feed composition, low energy consumption and low separation cost. WO2003010125 uses an impregnation method to prepare a nickel (26-65wt%) supported alumina catalyst, and uses ethylenediamine as a raw material to catalyze the synthesis of di...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C209/64C07C211/14
CPCB01J23/002B01J23/894B01J23/8953B01J2523/00C07C209/64B01J2523/17B01J2523/31B01J2523/3706B01J2523/824B01J2523/845B01J2523/847B01J2523/3712B01J2523/27C07C211/14
Inventor 张前杨建明赵锋伟余秦伟王为强梅苏宁李亚妮袁俊惠丰吕剑
Owner XIAN MODERN CHEM RES INST
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