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Dimethyl ethanolamine catalytic hydrogenation catalyst and preparation method thereof

A dimethylethanolamine, catalytic hydrogenation technology, applied in the preparation of amino compounds, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve processing difficulties, discharge pollution to the environment, increase production Cost and other issues, to achieve the effect of simple preparation method, low price and long service life

Inactive Publication Date: 2016-06-01
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above two patented processes are simple, easy to realize continuous industrial production, and the yield is high, but the main problem is that a large amount of waste water containing inorganic salts is generated during the process of adding alkali to the reaction solution to recover excess dimethylamine, which is difficult to treat and pollutes the discharge. environment, complete processing increases production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 96.2g of Cu(NO 3 ) 2 .3H 2 O and 14.1g of Ni(NO 3 ) 2 .6H 2 O was dissolved in 110ml of distilled water. After it was completely dissolved, 50g of diatomaceous earth was added and impregnated for 4 hours at a temperature of 80°C. The dried catalyst was ground into powder, and then placed in a muffle furnace and roasted at 450°C for 8 hours to obtain a catalyst precursor, in which the mass percentage of the active component was 15%, and the mass percentage of the carrier was 85%. Press the calcined catalyst into tablet form, cut and screen 20ml of catalyst with 20-40 mesh, and then reduce and activate the obtained catalyst. .

[0020] Adopt this catalyst to carry out the fixed-bed reaction of dimethylethanolamine and dimethylamine synthesis tetramethylethylenediamine, by gas chromatography analysis product composition, the conversion rate of dimethylethanolamine is 85.2%, the selection of tetramethylethylenediamine The specificity is 86.3%, and the catalyst ...

Embodiment 2

[0022] Weigh 126.3g of Cu(NO 3 ) 2 .3H 2 O, 20.1g Ni(NO 3 ) 2 .6H 2 O and 14.3g of Cr(NO 3 ) 3 .9H 2 O was dissolved in 100ml of distilled water. After it was completely dissolved, an equal volume of the solution was added to 50g of silicon spheres, sealed and impregnated at room temperature for 48 hours. Hours, and then placed in a muffle furnace for 3 hours at 650 ° C to roast to obtain a catalyst precursor, wherein the mass percentage of the active component is 35%, and the mass percentage of the carrier is 65%. The obtained catalyst was then reductively activated under the following conditions: reduction with hydrogen (hydrogen pressure: 2.0Mpa) at 250°C for 12 hours.

[0023] Adopt this catalyst to carry out the fixed-bed reaction of dimethylethanolamine and dimethylamine to synthesize tetramethylethylenediamine, by gas chromatography analysis product composition, the transformation rate of dimethylethanolamine is 93.2%, the selection of tetramethylethylenediamine...

Embodiment 3

[0025] Weigh 120.1g of Cu(NO 3 ) 2 .3H 2 O, 8.3g of Ni(NO 3 ) 2 .6H 2 O and 17.2g of Ba(NO 3 ) 2 Dissolve in 100ml of distilled water. After completely dissolving, add an equal volume of this solution into 50g of γ-alumina balls, seal and impregnate at room temperature for 24 hours, blot the excess solution after impregnation, and place in an oven at 110°C Dry in medium for 12 hours, and then place it in a muffle furnace and bake at 450°C for 5 hours to obtain a catalyst precursor, in which the mass percentage of the active component is 31%, and the mass percentage of the carrier is 69%. The obtained catalyst was then reductively activated under the following conditions: reduction with hydrogen (hydrogen pressure: 0.3Mpa) at 300°C for 7 hours.

[0026] Adopt this catalyst to carry out the fixed-bed reaction of dimethylethanolamine and dimethylamine to synthesize tetramethylethylenediamine, by gas chromatography analysis product composition, the transformation rate of di...

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Abstract

The invention relates to a dimethyl ethanolamine catalytic hydrogenation catalyst and a preparation method thereof, and belongs to the technical field of preparation of hydrogenation catalysts. The catalyst comprises an active component and a carrier, wherein the weight percentage content of the active component is 10-55 percent, the weight percentage content of the carrier is 45-90 percent, and the sum of the weight percentage contents is 100 percent. The active component of the catalyst is nickel or / and copper or / and chromium or / and zinc or / and iron or / and barium or / and aluminum or / and cobalt; the catalyst carrier is a silicon ball, an alumina ball, nanometer aluminum oxide, diatomite, activated carbon, ZSM-5 and the like. The preparation method provided by the invention is simple, convenient, low in cost and easy to industrialize; the service life of the catalyst is longer; the prepared catalyst has higher conversion rate and selectivity.

Description

Technical field: [0001] The invention belongs to the technical field of hydrogenation catalyst preparation, in particular to a dimethylethanolamine catalytic hydrogenation catalyst and a preparation method. Background technique: [0002] N, N, N', N'-Tetramethylethylenediamine is a colorless transparent liquid with a slight ammonia smell, miscible with water and most organic solvents such as ethanol, and is an important organic intermediate , mainly used as biochemical reagents, epoxy resin crosslinking agents, synthetic intermediates of quaternary ammonium compounds. [0003] The most traditional industrial method for preparing N,N,N',N'-tetramethylethylenediamine is to react with ethylenediamine with formic acid and formaldehyde as methylating reagents, formaldehyde provides methyl, and formic acid provides hydrogen protons And as a reducing agent, this method has mild reaction conditions, can be produced under normal temperature and pressure, and has a high conversion ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/86B01J23/78B01J23/80C07C209/16C07C211/10
CPCB01J23/755B01J21/04B01J21/16B01J23/78B01J23/80B01J23/86C07C209/16C07C211/10
Inventor 何明阳吴军钱俊峰陈群
Owner CHANGZHOU UNIV
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