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Method for preparing alkylamine ester oxalate

A technology of oxalic acid and CH2, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., can solve problems such as easy damage, product structure and performance changes, and achieve low cost and high yield.

Inactive Publication Date: 2013-06-19
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vinylamine itself has high activity, and the existing process is easily destroyed during the reaction process, resulting in changes in product structure and performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1H2

[0025] Example 1H 2 N(CH 2 ) 3 OCOCOO (CH 2 ) 3 NH 2 The preparation process

[0026] (1) Esterification

[0027] Add 150g of 100% propanolamine to the reaction tank, add 90g of 100% oxalic acid in 50 minutes at a temperature of less than 30°C, raise the temperature to 50°C, keep the temperature at 50°C, and react for 5 hours. to room temperature, set aside.

[0028] (2) Freezing

[0029] Add the resulting esterified stream into a reaction tank with direct ice, maintain the temperature at -5 to 15°C with direct ice until all of it is added, and part of the material is separated out for later use.

[0030] (3) filter

[0031] The filter cake is collected in the solid-liquid separator, and the mother liquor is recycled because it contains acid.

[0032] (4) Neutralization

[0033] The filter cake was dissolved in water, then sprayed and dried to obtain 136.86g of H 2 N(CH 2 ) 3 OCOCOO (CH 2 ) 3 NH 2

Embodiment 2H2

[0034] Example 2H 2 NCH 2 OCOCOO (CH 2 ) 2 NH 2 The preparation process of .

[0035] (1) Esterification

[0036] Add 47g of 100% methanolamine and 61g of 100% ethanolamine to the reaction tank, add 90g of 100% oxalic acid in 50 minutes at a temperature of less than 30°C, raise the temperature to 50°C, and keep the temperature at 50°C. React for 5 hours, cool down to room temperature, and set aside.

[0037] (2) Freezing

[0038] Add the resulting esterified stream into a reaction tank with direct ice, maintain the temperature at -5 to 15°C with direct ice until all of it is added, and part of the material is separated out for later use.

[0039] (3) filter

[0040] The filter cake is collected in the solid-liquid separator, and the mother liquor is recycled because it contains acid.

[0041] (4) Neutralization

[0042] The filter cake was dissolved in water, then sprayed and dried to obtain 145.8g of H 2 NCH 2 OCOCOO (CH 2 ) 2 NH 2 ..

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PUM

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Abstract

The invention provides a method for preparing alkylamine ester oxalate, which comprises the following steps: adding water solution of H2N(CH2)nOH and H2N(CH2)mOH into a reaction tank, adding oxalic acid under the condition that the temperature is lower than 30 DEG C, increasing the temperature to 50 DEG C, keeping the temperature at 50-60 DEG C, reacting for 4-6h, reducing the temperature to the room temperature, adding an obtained ester small stream into the reaction tank with direct ice, keeping the temperature at minus 5 DEG C to 15 DEG C, adding all the materials, partially precipitating the materials, then filtering and dissolving, thereby obtaining a product of H2N(CH2)nOCOCOO(CH2)mNH2.

Description

technical field [0001] The invention belongs to the field of intermediate product preparation of synthetic dyes, in particular to a preparation method of alkylamine oxalate. Background technique [0002] Alcohol amine ester compound is a new type of dye intermediate, and its raw materials are alcohol amine and oxalic acid. There are many methods available for the preparation of alcohol amine esters, which include a variety of methods. However, due to the difficulty in post-esterification treatment, low conversion rate of esterification and dangerous operation, this patent selects the oleum esterification method. The raw material of this method is easy to obtain, and the manufacturing process is simple and easy to implement. During the preparation process, since the alcohol amine itself has a certain volatility, it is necessary to add a reflux device to prevent the inaccurate proportioning caused by the loss of materials during the reaction. Moreover, it has been found thr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/06C07C227/08
Inventor 张兴华郝津来
Owner TIANJIN DEK CHEM
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