A kind of method for preparing pentamethyldipropylene triamine

A technology of pentamethyldipropylenetriamine and dimethylaminopropylamine, which is applied to the preparation of amino compounds from amines, carboxylic acid nitriles, amino compounds, etc., and can solve the problem of many by-products, difficult hydrogenation, and raw material methylamine. Great odor and other problems, to achieve the effect of reducing the formation of by-products, reasonable acid distribution, and accelerated hydrogenation speed

Active Publication Date: 2022-08-05
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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  • A kind of method for preparing pentamethyldipropylene triamine
  • A kind of method for preparing pentamethyldipropylene triamine
  • A kind of method for preparing pentamethyldipropylene triamine

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Preparation of 1# modified carrier:

[0052] The 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 , 1g Nb 2 O 5 immersion solution, then heated to 90 °C to form a homogeneous solution, 94 g of γ-Al 2 O 3 Add it to the dipping solution, immerse it at 90°C for 12h, bake it in a 120°C oven for 12h; finally move it to a muffle furnace, heat it up to 500°C for 8 hours at 3°C / min in an air atmosphere, and obtain a mass Fraction is 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] Prepare a nitrate impregnation solution containing 4g palladium, 1g zinc and 0.3g rhenium with 80ml deionized water, heat to 80°C to form a homogeneous solution, add 94.7g 1# modified carrier, impregnate it at 80°C for 8h, and then immerse it at 120°C for...

Embodiment 2

[0056] Preparation of 2# modified carrier:

[0057] The 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 dipping solution, then heated to 80 °C to form a homogeneous solution, 89.5 g of γ-Al 2 O 3 Add it to the dipping solution, soak it at 80°C for 16h, bake it in an oven at 110°C for 8h; finally move it to a muffle furnace, heat it up to 450°C for 8 hours at 2°C / min in an air atmosphere, and obtain a mass 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] Prepare a nitrate impregnation solution containing 10g palladium, 0.5g zinc and 0.2g rhenium with 100ml deionized water, heat it to 90°C to form a homogeneous solution, add 89.3g 2# modified carrier, soak it at 90°C for 24h, and then Bake in an oven...

Embodiment 3

[0061] 3# Modified carrier preparation:

[0062] The 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 dipping solution, then heated to 85 °C to form a homogeneous solution, 93 g of γ-Al 2 O 3 Add it to the immersion solution, soak it at 85°C for 24h, bake it in an oven at 100°C for 12h; finally move it to a muffle furnace, heat it up to 300°C for 8 hours at 2°C / min in an air atmosphere, and 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] Prepare a nitrate impregnation solution containing 2g palladium, 0.8g molybdenum and 1g chromium with 50ml deionized water, heat to 90°C to form a homogeneous solution, then add 96.2g 3# modified carrier, impregnate it at 90°C for 8h, then at 110°C Bake in a...

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Abstract

The invention provides a method for preparing pentamethyldipropylene triamine. The method comprises the following steps: (1) 3-dimethylaminopropylamine and acrylonitrile are reacted to generate 3-[[3-(dimethylamino)propyl]amino]propionitrile reaction solution, and 3-[[3 -(dimethylamino)propyl]amino]propionitrile pure product; (2) adding 3-[[3-(dimethylamino)propyl]amino]propionitrile to hydrogen and solvent under the action of a catalyst; Hydrogen reaction obtains N'-(3-aminopropyl)-N,N-dimethyl-1,3-propanediamine reaction solution; (3) N'-(3-aminopropyl) obtained in step (2) base)-N,N-dimethyl-1,3-propylenediamine reaction solution and formaldehyde and hydrogen undergo methylation reaction under the action of a catalyst to obtain pentamethyldipropylenetriamine. The method has the advantages of cheap and easy-to-obtain starting materials, good product selectivity, high product yield, economical and effective method, and industrialization prospect.

Description

technical field [0001] The invention relates to a preparation method of a polyurethane catalyst, and more particularly to a preparation method of pentamethyldipropylene triamine. Background technique [0002] Pentamethyldipropylene triamine is a balanced polyurethane foaming catalyst, which is widely used in the field of flexible and rigid foam, and has been used in the field of polyurethane for a long time. Its characteristics are: 1. catalyzes foaming and gelation reactions; 2. provides more open-cell foam; 3. produces softer foam in high-water formulations; 4. reduces Foam peeling; 5. In terms of hard foam, it can reduce the fragility of the foam and improve the adhesion. [0003] There are few production routes of pentamethyldipropylene triamine reported in the literature at present, there are mainly two routes, the first route is Liang, Hong-Chang (Journal of the American Chemical Society, 124(16), 4170-4171) 2002 The Eschweiler-Clarke reaction that reported in 2010 g...

Claims

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Application Information

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Patent Type & Authority Patents(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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