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Synthesis method of 3-methoxypropylamine

A technology for the synthesis of methoxypropylamine and its synthesis method, which is applied in the field of synthesis of 3-methoxypropylamine, can solve the problems of low yield of main product, increased production cost, increased processing difficulty, energy consumption and material consumption, etc., and achieves reduction of methanol consumption , improve the conversion rate and storage time, and improve the effect of selectivity

Pending Publication Date: 2022-04-05
WANHUA CHEM GRP CO LTD
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  • Application Information

AI Technical Summary

Problems solved by technology

However, although this scheme reduces the content of acrylonitrile in 3-methoxypropionitrile to 0, the hydrogenation reaction stage will still inevitably generate n-propylamine due to the addition of basic additives; on the other hand, 3-methoxypropionitrile The crude product of propionitrile increases processing difficulty and energy and material consumption through refining, causes production cost to increase
[0005] Chinese patent CN 109369423 A discloses a method for preparing 3-ethoxypropylamine. Its process route is similar to that of 3-methoxypropylamine. The hydrogenation reaction uses a large amount of liquid ammonia to suppress the formation of secondary amine by-products, but a large amount of liquid ammonia The introduction of 3-ethoxypropionitrile will inevitably cause the decomposition of intermediate 3-ethoxypropionitrile to produce acrylonitrile, and further hydrogenation will produce a large amount of by-product n-propylamine, so the highest yield of the main product 3-ethoxypropylamine is only 94.6%
[0006] In summary, there are problems in the prior art that the content of the by-product n-propylamine cannot be significantly reduced and the yield of the main product is low. Therefore, there is still a need for a new synthetic method for 3-methoxypropylamine, which can efficiently synthesize 3- Methoxypropylamine can effectively reduce the generation of hydrogenation reaction by-products, greatly simplifying the synthesis process

Method used

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  • Synthesis method of 3-methoxypropylamine

Examples

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preparation example Construction

[0026] A kind of synthetic method of 3-methoxypropylamine, comprises the following steps:

[0027] (1) Using acrylonitrile and methanol as raw materials and an alkaline buffer as an auxiliary agent, acrylonitrile is added dropwise to a methanol solution containing an alkaline buffer to react to synthesize the crude product of 3-methoxypropionitrile;

[0028] (2) Using the crude product of 3-methoxypropionitrile as a raw material, in the presence of a solvent and a catalyst, the crude product of 3-methoxypropylamine is synthesized by catalytic hydrogenation.

[0029] (3) Carry out rectification to the 3-methoxypropylamine crude product, obtain the 3-methoxypropylamine product of purity>99.0%, and reclaim solvent methanol.

[0030] In the step (1), the alkaline buffer is ammonium carbonate-ammonium bicarbonate aqueous solution, and the total mass concentration of ammonium carbonate / ammonium bicarbonate is 0.1-10wt%, for example including but not limited to 0.1wt%, 0.5wt%, 1wt% ...

Embodiment 1

[0043] A kind of synthetic method of 3-methoxypropylamine, comprises the following steps:

[0044] (1) Weigh 0.096g of ammonium carbonate and 0.016g of ammonium bicarbonate and dissolve them in 1g of deionized water, combine them with 158g of methanol, and then transfer them to a 1L reaction kettle. After the kettle is combined, replace it with nitrogen three times, and then pressurize the nitrogen to 0.5MPa. Turn on stirring and heating. After the temperature in the reaction kettle rises to 35°C, use a convection pump for 0.15h -1 Acrylonitrile was fed at volumetric space velocity, and the reaction temperature was maintained at 35°C. When the feed amount of acrylonitrile reaches 174.5 g, the feed is stopped, the temperature is maintained and the reaction is prolonged for 1 h to finally obtain the crude product of 3-methoxypropionitrile. According to GC chromatographic analysis, the residual amount of acrylonitrile in the reaction solution was 0.15%, and the yield of 3-metho...

Embodiment 2

[0048] (1) Weigh 0.096g of ammonium carbonate and 0.008g of ammonium bicarbonate and dissolve them in 3.4g of deionized water, combine them with 158g of methanol and transfer them to a 1L reactor. After the reactor is combined, replace it with nitrogen three times, and then pressurize the nitrogen to 0.5MPa. Turn on stirring and heating. After the temperature in the reactor rises to 30°C, use a convection pump to -1 Acrylonitrile was fed at space velocity and the reaction temperature was maintained at 30°C. When the feed amount of acrylonitrile reaches 174.5 g, the feed is stopped, the reaction temperature is maintained and the reaction is prolonged for 1 h. Finally, the crude product of 3-methoxypropionitrile was obtained. According to GC chromatographic analysis, the residual amount of acrylonitrile in the reaction solution was 0.2%, and the yield of 3-methoxypropionitrile was 99.7%.

[0049] (2) The Raney cobalt catalyst with a wet weight of 2g is transferred to the auto...

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Abstract

The invention discloses a synthesis method of 3-methoxypropylamine, which comprises the following steps: carrying out addition reaction on methanol and acrylonitrile to synthesize a 3-methoxypropionitrile crude product, and then carrying out catalytic hydrogenation on the 3-methoxypropionitrile crude product to synthesize the 3-methoxypropylamine. In the addition reaction, an ammonium carbonate-ammonium bicarbonate buffer solution is used as an auxiliary agent, so that the acrylonitrile conversion rate can be greater than or equal to 99.5%; the obtained addition reaction crude product does not need to be neutralized and is directly hydrogenated, the yield of the 3-methoxypropylamine is greater than or equal to 95.5%, the content of the by-product n-propylamine is not higher than 0.2%, and the recovery rate gt of the solvent methanol; 95%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of 3-methoxypropylamine. Background technique [0002] 3-Methoxypropylamine (MOPA) is a primary amine compound with wide application, mainly used as mineral flotation agent, and has higher selectivity for iron ore flotation than ordinary surfactants. In addition, 3-methoxypropylamine can be used as an important intermediate for the synthesis of dyes such as disperse green blue S-GL, and is also widely used in the formulation of metal corrosion inhibitors. The dosage of the formulation accounts for about 5-15% of the total formulation quality. Corrosion inhibitors are gradually popularized and used in the petrochemical industry, so they have a good application prospect. [0003] The mainstream synthetic route of 3-methoxypropylamine is the addition hydrogenation method, that is, acrylonitrile (ACN) and methanol synthesize 3-methoxypropioni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C217/08C07C253/30C07C255/13
Inventor 姜瑞航张聪颖刘振国
Owner WANHUA CHEM GRP CO LTD
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