阅读说明：本技术 一种甲氧基丙胺的合成工艺 (Synthesis process of methoxypropylamine ) 是由 刘涛 李福同 庞宝阳 张娟 于 2021-07-26 设计创作，主要内容包括：本发明公开了一种甲氧基丙胺的合成工艺,其特征在于,包括以下步骤：(1)以3-甲氧基丙腈为原料,将3-甲氧基丙腈、溶剂、改性剂和催化剂放入高压釜中,对催化剂进行改性；(2)在特定温度下,真空向高压釜中通入甲胺/碱金属氢氧化物,再通氢气,加热到一定温度,并维持压强在2-3MPa下进行搅拌反应2h后,得到搅拌液；反应结束后将高压釜降至室温,然后对高压釜内的搅拌液进行过滤,过滤后常压下进行精馏,得到无色透明的3-甲氧基丙胺。与现有技术相比,本发明以3-甲氧基丙腈为原料,催化加氢；本方法的工艺流程简单,转化率高,选择性好。(The invention discloses a synthesis process of methoxypropylamine, which is characterized by comprising the following steps: (1) 3-methoxypropionitrile is taken as a raw material, and the 3-methoxypropionitrile, a solvent, a modifier and a catalyst are put into a high-pressure kettle to modify the catalyst; (2) introducing methylamine/alkali metal hydroxide into the high-pressure kettle in vacuum at a specific temperature, introducing hydrogen, heating to a certain temperature, and stirring and reacting for 2 hours under the pressure of 2-3MPa to obtain a stirring liquid; and (3) after the reaction is finished, cooling the autoclave to room temperature, filtering the stirred solution in the autoclave, and rectifying under normal pressure after filtering to obtain colorless and transparent 3-methoxypropylamine. Compared with the prior art, the method takes 3-methoxypropionitrile as a raw material and carries out catalytic hydrogenation; the method has the advantages of simple process flow, high conversion rate and good selectivity.)

1. A synthesis process of methoxypropylamine is characterized by comprising the following steps:

(1) 3-methoxypropionitrile is taken as a raw material, and the 3-methoxypropionitrile, a solvent, a modifier and a catalyst are put into a high-pressure kettle to modify the catalyst;

(2) adding methylamine/alkali metal hydroxide into an autoclave in vacuum at room temperature, then adding hydrogen, heating to a certain temperature, and stirring and reacting for 2 hours under the pressure of 0.2-3MPa to obtain a stirring liquid;

(3) and (3) after the reaction is finished, cooling the autoclave to room temperature, filtering the stirred solution in the autoclave, and rectifying under normal pressure after filtering to obtain colorless and transparent 3-methoxypropylamine.

2. The process of claim 1, wherein the catalyst is one or more of a nickel-aluminum catalyst, a cobalt-aluminum catalyst, a palladium and platinum-aluminum catalyst, a copper-chromium catalyst, a rhodium catalyst, and a ruthenium catalyst.

3. The process of claim 2, wherein the modifier is one of sodium dihydrogen phosphate, sodium hydrogen sulfate, phosphoric acid, a mixture of phosphoric acid and phosphate, acetic acid, a mixture of acetic acid and acetate, citric acid, and sodium hydrogen citrate.

4. The process for synthesizing methoxypropylamine according to claim 2, wherein the amount of the catalyst is 0.1-15% by mass of the raw material.

5. The process for synthesizing methoxypropylamine according to claim 1, wherein the amount of methylamine/alkali metal hydroxide is 0.1-15% by mass of the raw materials.

6. The process for synthesizing methoxypropylamine according to claim 1, wherein the temperature is controlled between 60 ℃ and 130 ℃.

7. The process for synthesizing methoxypropylamine according to claim 1, wherein the amount of the solvent is 1% -10% by mass of the raw materials.

8. The process for synthesizing methoxypropylamine according to claim 1, wherein the solvent is one of ethanol, isopropanol, toluene, and water.

Technical Field

The invention relates to the technical field of synthesis of methoxypropylamine, and particularly relates to a synthesis process of methoxypropylamine.

Background

The existing synthesis method of methoxypropylamine is characterized in that 3-methoxypropanol is used as a raw material, Cu-Co/Al2O 3-diatomite is used as a catalyst, under the conditions of certain pressure and temperature, 3-methoxypropionitrile is thrown into a preheater, alkali metal hydroxide and hydrogen are mixed, preheated and vaporized, then the mixture enters a fixed bed reactor for reaction, after the reaction, the material is subjected to condensation cooling and gas-liquid separation, 3-methoxypropylamine is taken out as a product, and the system material is recycled.

Disclosure of Invention

In view of the above, the present invention aims to provide a synthesis process of methoxypropylamine, which is simple to operate and has significantly improved conversion rate and reaction selectivity.

In order to achieve the purpose, the invention provides the following technical scheme:

a synthesis process of methoxypropylamine is characterized by comprising the following steps:

(1) 3-methoxypropionitrile is taken as a raw material, and the 3-methoxypropionitrile, a solvent, a modifier and a catalyst are put into a high-pressure kettle to modify the catalyst;

(2) adding methylamine/alkali metal hydroxide into an autoclave in vacuum at room temperature, then adding hydrogen, heating to a certain temperature, and stirring and reacting for 2 hours under the pressure of 0.2-3MPa to obtain a stirring liquid;

(3) and (3) after the reaction is finished, cooling the autoclave to room temperature, filtering the stirred solution in the autoclave, and rectifying under normal pressure after filtering to obtain colorless and transparent 3-methoxypropylamine.

In the synthesis process of the methoxypropylamine, the catalyst is one of a nickel catalyst, a cobalt catalyst, a palladium and platinum catalyst, a copper-chromium catalyst, a rhodium catalyst and a ruthenium catalyst; preferably, the catalyst is a nickel catalyst and a cobalt catalyst; preferably, the catalyst is a nickel catalyst.

In the synthesis process of the methoxypropylamine, the modifier is one of sodium dihydrogen phosphate, sodium bisulfate, phosphoric acid, a mixture of phosphoric acid and phosphate, acetic acid, a mixture of acetic acid and acetate, citric acid and sodium hydrogen citrate.

In the synthesis process of the methoxypropylamine, the dosage of the catalyst is 1-20% of the mass of the raw material; preferably, the dosage of the catalyst is 3-15% of the mass of the raw materials; preferably, the dosage of the catalyst is 3-10% of the mass of the raw materials.

In the synthesis process of the methoxypropylamine, the dosage of the methylamine/alkali metal hydroxide is 5-25% of the mass of the raw materials. Preferably, the dosage of the methylamine/alkali metal hydroxide is 5-15% of the mass of the raw materials. Preferably, the dosage of the methylamine/alkali metal hydroxide is 7-10% of the mass of the raw materials.

In the synthesis process of the methoxypropylamine, the temperature is controlled between 60 and 150 ℃. Preferably, the temperature is controlled between 70 and 120 ℃. Preferably, the temperature is controlled between 90 ℃ and 110 ℃.

In the synthesis process of the methoxypropylamine, the dosage of the solvent is 1-10% of the mass of the raw materials. Preferably, the amount of the solvent is 1-5% of the mass of the raw materials. Preferably, the amount of the solvent is 1-2% of the mass of the raw materials.

In the synthesis process of the methoxypropylamine, the temperature is controlled between 60 and 150 ℃. Preferably, the temperature is controlled between 70 and 120 ℃. Preferably, the temperature is controlled between 90 ℃ and 110 DEG C

According to the technical scheme, compared with the prior art, the method takes the 3-methoxypropionitrile as the raw material to carry out catalytic hydrogenation; the method has the advantages of simple process flow, high conversion rate, good selectivity, wide selection range of the catalyst, wide controllable condition range and contribution to large-scale production regulation and control.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

a synthesis method of 3-methoxypropylamine takes 3-methoxypropionitrile as a raw material for catalytic hydrogenation:

400g of 3-methoxypropionitrile, 20g of ethanol and 12g of a modified supported nickel catalyst were placed in a 1000ml autoclave; introducing 40g of monomethylamine at room temperature in vacuum, introducing hydrogen to 2.0MPa, heating to 90 ℃, maintaining the pressure at 2.8MPa, stirring for reaction for 2 hours, cooling to room temperature after the reaction is finished, filtering the kettle liquid, and rectifying at normal pressure (collecting 110-160 ℃ fraction) to obtain 354.09g of colorless and transparent 3-methoxypropylamine. After the reaction was completed, the reaction residue was analyzed by gas chromatography to obtain a raw material conversion of 97.0% and a product yield of 94.52%.

Example 2 to example 6:

the amount of the catalyst used in example 1 was adjusted, and the remaining conditions were identical to those in example 1, and the conversion and the total yield of the raw materials were obtained as shown in the following table.

Implementation plan	1	2	3	4	5	6
							Catalyst addition/g	12	0.4	4	20	40	60
Raw material conversion/%	97	95.2	96.21	97.23	97.15	97.02
							Product yield/%	94.52	92.11	91.68	95.43	95.11	95.86

Example 7 to example 10:

the temperature and pressure conditions in example 1 were adjusted, and the remaining conditions were identical to those in example 1, and the conversion and total yield of the raw materials were obtained as shown in the following table.

Example sequence number	1	7	8	9	10
						Temperature/. degree.C	90	60	130	90	90
Pressure intensity/MPa	2.80	2.80	2.80	2.00	3.00
						Raw material conversion/%	97	95.56	97.73	95.11	97.13
Product yield/%	94.52	92.83	94.44	92.55	94.87

Example 11 to example 13:

the amount of methylamine used in example 1 was adjusted, and the remaining conditions were the same as in example 1, and the conversion and total yield of the raw materials were as shown in the following table.

Example sequence number	1	11	12	13
					Methylamine/g	40	0.4	10	60
Raw material conversion/%	97	88.55	94.21	97.78
					Product yield/%	94.52	83.24	91.11	95.11

Example 11 to example 13:

the kind and amount of the solvent used in example 1 were adjusted, and the remaining conditions were identical to those in example 1, and the conversion and total yield of the raw materials were as shown in the following table.

Example sequence number	1	14	15	16	17	18
							Ethanol/g	20
Isopropyl alcohol/g		20
							Water/g			20		10	30
Toluene/g				20
							Raw material conversion/%	97	96.55	97.21	96.78	95.88	95.39
Product yield/%	94.52	94.24	95.11	95.11	94.25	94.69

From the data in the above three tables, it can be seen that under the process conditions of the present inventors, both higher conversions and higher product yields are obtained.

Example 19:

putting 1500kg of 3-methoxypropionitrile, 45kg of water and 45kg of modified catalyst into a high-pressure kettle, introducing 150kg of methylamine at normal temperature under vacuum, introducing hydrogen to 2.00MPa, heating to 100 ℃, maintaining the pressure at 2.70MPa, stirring for reaction, reducing the reaction temperature to room temperature after the reaction is finished, filtering the kettle liquid, and rectifying at normal pressure (collecting 110-160 ℃ fraction) to obtain 1253kg of colorless and transparent 3-methoxypropylamine. The gas chromatography analysis of the residue after the completion of the reaction gave a raw material conversion of 97.86% and a product yield of 94.53%.

The reaction mechanism of the invention is as follows:

the embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.