Method for preparing pentamethyldipropylene triamine

A technology for pentamethyldipropylenetriamine and dimethylaminopropylamine, which is applied in the preparation of amino compounds from amines, the preparation of carboxylic acid nitrile, the preparation of amino compounds, etc., can solve the problems of many by-products, difficult hydrogenation, and raw material methylamine. odor and other problems, to achieve the effect of accelerating hydrogenation rate, reasonable acidity distribution, and improving dispersion effect

Active Publication Date: 2019-11-12
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The advantage of this method is that the raw materials are relatively cheap, and the disadvantages are: 1. The product of the first step is dicyanide, so the hydrogenation difficulty of the second step is relatively large, and there are many by-products, which are mainly aminonitrile and diimine according to literature reports. , piperazines, under optimal conditions, the selectivity of N-(3-aminopropyl)-N-methylpropane-1,3-diamine is only 85%, and the yield of the final product is only 67%. %; 2. In addition, each step of this method is not separated, which will cause the separation difficulty of the product to increase; 3. The odor of the raw material methylamine is relatively large, which is likely to cause environmental problems; Complex, low degree of automation, high labor intensity, high probability of safety accidents
[0009] Therefore, it is necessary to find a new production method of pentamethyldipropylenetriamine to solve the problems of high raw material cost, low product yield and difficult separation of impurities in the traditional process

Method used

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  • Method for preparing pentamethyldipropylene triamine
  • Method for preparing pentamethyldipropylene triamine
  • Method for preparing pentamethyldipropylene triamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Preparation of 1# modified carrier:

[0052] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 280m 2 / g) Calcined at 450°C for 4h. Prepare ammonium fluorosilicate and niobium nitrate with 100ml deionized water containing 5g SiO 2 , 1 g Nb 2 o 5 The immersion solution, and then heated to 90 ° C to form a uniform solution, 94g γ-Al 2 o 3 Add it to the impregnation solution, impregnate it at 90°C for 12 hours, bake it in an oven at 120°C for 12 hours; finally move it to a muffle furnace, heat it up to 500°C at 3°C / min and bake it for 8 hours in an air atmosphere to obtain a mass containing Fraction 5% SiO 2 +1%Nb 2 o 5 +94%γ-Al 2 o 3 modified carrier.

[0053] Preparation of 1# supported palladium-based catalyst precursor:

[0054] Use 80ml of deionized water to prepare a nitrate impregnation solution containing 4g of palladium, 1g of zinc, and 0.3g of rhenium, heat it to 80°C to form a homogeneous solution, then add 94.7g of 1# modified carrier...

Embodiment 2

[0056] Preparation of 2# modified carrier:

[0057] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 280m 2 / g) Calcined at 400°C for 8h. Prepare ammonium fluorosilicate and niobium nitrate with 120ml deionized water containing 10g SiO 2 , 0.5g Nb 2 o 5 immersion solution, and then heated to 80 ° C to form a uniform solution, 89.5g γ-Al 2 o 3 Add it to the impregnation solution, impregnate it at 80°C for 16 hours, bake it in an oven at 110°C for 8 hours; finally move it to a muffle furnace, heat it up to 450°C at 2°C / min and bake it for 8 hours in an air atmosphere to obtain a mass containing Fraction 10% SiO 2 +0.5%Nb 2 o 5 +89.5%γ-Al 2 o 3 modified carrier.

[0058] Preparation of 2# supported palladium-based catalyst precursor:

[0059] Use 100ml of deionized water to prepare a nitrate impregnation solution containing 10g of palladium, 0.5g of zinc, and 0.2g of rhenium, heat it to 90°C to form a homogeneous solution, then add 89.3g of 2# modified...

Embodiment 3

[0061] Preparation of 3# modified carrier:

[0062] Spherical γ-Al 2 o 3 (particle size 3mm, specific surface area 280m 2 / g) Calcined at 500°C for 4h. Prepare ammonium fluorosilicate and niobium nitrate with 80ml deionized water containing 2g SiO 2 , 5g Nb 2 o 5 immersion solution, and then heated to 85 ° C to form a homogeneous solution, 93g γ-Al 2 o 3 Add to the impregnating solution, impregnate at 85°C for 24h, bake in an oven at 100°C for 12h; finally move to a muffle furnace, heat up to 300°C at 2°C / min and bake for 8 hours in an air atmosphere to obtain the mass fraction 2% SiO 2 +5%Nb 2 o 5 +93%γ-Al 2 o 3 modified carrier.

[0063] Preparation of 3# supported palladium-based catalyst precursor:

[0064] Use 50ml of deionized water to prepare a nitrate dipping solution containing 2g of palladium, 0.8g of molybdenum, and 1g of chromium, heat it to 90°C to form a homogeneous solution, then add 96.2g of 3# modified carrier, immerse at 90°C for 8h, and then at...

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Abstract

The invention provides a method for preparing pentamethyldipropylene triamine. The method comprises the following steps: (1) performing a reaction on 3-dimethylaminopropylamine and acrylonitrile so asto form a 3-[[3-(dimethylamino)propyl]amino]propionitrile reaction solution, and performing separation so as to obtain a 3-[[3-((dimethylamino)propyl]amino]propionitrile pure product; (2) performinga hydrogenation reaction on 3-[[3-(dimethylamino)propyl]amino]propionitrile, hydrogen and a solvent under the action of a catalyst so as to obtain a N'-(3-aminopropyl)-N,N-dimethyl-1,3-propylene diamine reaction solution; and (3) performing a methylation reaction on the N'-(3-aminopropyl)-N,N-dimethyl-1,3-propylene diamine reaction solution obtained in the step (2), formaldehyde and hydrogen underthe action of a catalyst so as to obtain pentamethyldipropylene triamine. The method has the advantages of cheap and easily available starting materials, good selectivity to the product and high product yield, and the method is economical and effective, and has industrialization prospects.

Description

technical field [0001] The present invention relates to a kind of preparation method of polyurethane catalyst, more specifically relate to a kind of preparation method of pentamethyldipropylene triamine. Background technique [0002] Pentamethyldipropylenetriamine is a balanced polyurethane foaming catalyst, which is widely used in soft foam and rigid foam fields, and has been used in polyurethane field for a long time. Its characteristics are: 1. Catalyze foaming and gel reaction; 2. Provide more open-cell foam; 3. Can produce softer foam in high water formula; 4. Can reduce foam in flexible foam molding foam Foam peeling; 5. In terms of hard foam, it can reduce the fragility of the foam and improve the adhesion. [0003] The production routes of pentamethyldipropylene triamine reported in literature are few at present, mainly contain two, the first route is Liang, Hong-Chang (Journal of the American Chemical Society, 124 (16), 4170-4171) 2002 The Eschweiler-Clarke reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/24C07C209/48C07C209/68C07C209/26C07C211/14B01J23/648B01J23/652
CPCC07C253/30C07C209/48C07C209/68C07C209/26B01J23/6484B01J23/6525C07C255/24C07C211/14Y02P20/52
Inventor 刘振国张聪颖李鑫任树杰王丛张立娟李文滨
Owner WANHUA CHEM GRP CO LTD
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