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Method for pipelined continuous production of n-n-propylacetamide

A n-propyl acetamide, pipeline technology, applied in the direction of chemical instruments and methods, carboxylic acid amide preparation, organic compound preparation, etc., can solve the problems of low yield and long time, and achieve high yield and high production capacity Big, backmixed small effects

Inactive Publication Date: 2018-12-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has mild reaction conditions, and the catalyst is cheap and easy to obtain; but the time is long and the yield is low

Method used

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  • Method for pipelined continuous production of n-n-propylacetamide
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  • Method for pipelined continuous production of n-n-propylacetamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1. A method for pipelined continuous production of N-n-propylacetamide using figure 1 The device shown in, takes ethyl acetate and n-propylamine as raw materials, and performs the following steps in sequence:

[0051] (1) Add 300 mL of ethyl acetate to the measuring cylinder 1, fully open the valves in the system (including needle valves 12-14 and valve 15), and use a large flow rate of 10 mL / min to fill the reaction coil 4 with ethyl acetate; The remaining ethyl acetate in 1 was recovered, and 450 mL of a mixed solution of ethyl acetate and n-propylamine was added as the raw material for the reaction. The molar ratio of ethyl acetate and n-propylamine was 1:1.

[0052] (2) Fill the system pressure (ie, the pressure in the reaction coil 4) to 3 MPa with nitrogen (at this time, the readings of the pressure gauge 9 and the pressure gauge 10 are both 3 MPa), and the valve 15 is closed. Turn on the oil bath 3, set the temperature to 170°C, turn on the stirring paddle 5,...

Embodiment 2

[0062] Example 2. A method for pipelined continuous production of N-n-propylacetamide,

[0063] The molar ratio of ethyl acetate and n-propylamine is 1:0.5;

[0064] Set the flow rate of 0.40-1.00mL / min at the plunger pump 2,

[0065] The rest is equivalent to Example 1.

[0066] Under different flow rate conditions, the reaction yield is shown in Table 2 below:

[0067] Table 2. Reaction results at 170℃, raw material ratio 1:0.5

[0068]

Embodiment 3

[0069] Example 3. A method for pipelined continuous production of N-n-propylacetamide,

[0070] The molar ratio of ethyl acetate and n-propylamine is 1:2;

[0071] Set the flow at the plunger pump 2 to 0.40-1.00mL / min;

[0072] The rest is equivalent to Example 1.

[0073] Under different flow rate conditions, the reaction yield is shown in Table 3 below:

[0074] Table 3. Reaction results at 170°C and 1:2 ratio of raw materials

[0075]

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Abstract

The invention discloses a method for continuously producing N-propyl acetamide in a channelization mode. A utilized channelization reaction production device comprises a reaction coil, an outlet of the reaction coil is connected with an inlet of a high-pressure tank through a cooling coil, and a valve is arranged at the position of an outlet of the high-pressure tank. The method comprises the following steps: 1) filling the reaction coil with acetate; 2) improving pressure in the reaction coil to 3+ / -0.2MPa through inert gas and adjusting temperature in the reaction coil as 170 to 200 DEG C; 3) utilizing a mixed solution of acetate and n-propylamine as a reaction raw material, sending the mixed solution into the reaction coil at a certain flow to be reacted, cooling an obtained reaction solution through the cooling coil, flowing the reaction solution into the high-pressure tank and switching on the valve to drain the reaction solution in the high-pressure tank out when a pressure in the high-pressure tank is higher than 5MPa; and 4) distilling the reaction solution drained out of the high-pressure tank to remove an unreacted raw material and a product of alcohol to obtain N-propyl acetamide.

Description

Technical field [0001] The invention belongs to the field of organic synthesis and relates to a method for pipelined continuous production of N-n-propylacetamide. Background technique [0002] N-n-propylacetamide (CAS: 5331-48-6), its molecular formula is C 5 H 11 NO, the relative sub-mass is 101.15, and the molecular structure is as follows: [0003] [0004] N-n-propylacetamide is an important amide organic synthesis intermediate, and it can also be used in organic synthesis as a high boiling point solvent with good solubility. [0005] The following production methods are currently reported: [0006] Method 1: Tao Chen, Gaofeng Zeng, Zhiping Lai, Kuowei Huan, Journal of Membrane Science, 2016, 515:212-218, informing that ethanol and n-propylamine are used as raw materials, and 1,4-dioxane, tetrahydrofuran or toluene are used as solvents , Milstein catalyst, potassium tert-butoxide, reacted in a palladium / silver ceramic membrane reactor at 140-160℃ for 5 hours. Depending on the rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C233/05
CPCC07C231/02C07C233/05
Inventor 钱超欧阳博陈新志
Owner ZHEJIANG UNIV
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