Process for synthesizing sec-butyl urea

A technology for sec-butyl urea and sec-butyl amine, which is applied in the field of synthesizing sec-butyl urea by a CO2 catalytic method, can solve the problems of low market value and high cost of potassium sulfate, and achieve the effects of high market value, simple method and cost reduction.

Inactive Publication Date: 2006-09-06
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the synthesis of sec-butyl urea in China, and it has been produced by sulfuric acid catalysis abroad, that is, potassium cyanate aqueous solution and sec-butylamine are used to synthesize sec-butyl urea...

Method used

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  • Process for synthesizing sec-butyl urea
  • Process for synthesizing sec-butyl urea

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dilute 8.2g of sec-butylamine with 45ml of water and put it in a four-necked flask, weigh 8.1g of potassium cyanate and dissolve it in 20ml of water, add it to the four-necked flask, stir and mix well. Infuse CO under normal pressure 2 gas, maintained at 30°C for 4 hours. Evaporate water and excess sec-butylamine, add 50ml of ethanol, filter while hot to obtain 4.5g of by-product potassium carbonate, evaporate and concentrate the filtrate to obtain 7.6g of product sec-butylurea, and the conversion rate per pass is 65.2%.

Embodiment 2

[0023] Dilute 7.3g of sec-butylamine with 20ml of water and put it in a four-necked flask, weigh 8.1g of potassium cyanate and dissolve it in 20ml of water, add it to the four-necked flask, stir and mix well. Infuse CO under normal pressure 2 gas, maintained at 55°C for 6 hours. Evaporate water and excess sec-butylamine, add 50ml of ethanol, filter while hot to obtain 3.8g of by-product potassium carbonate, and evaporate and concentrate the filtrate to obtain 6g of product sec-butylurea, with a single-pass conversion rate of 51.7%.

Embodiment 3

[0025] Dilute 8.2g of sec-butylamine with 30ml of water and put it in a four-necked flask, weigh 8.1g of potassium cyanate and dissolve it in 20ml of water, add it to the four-necked flask, stir and mix well. Inject CO at 10 atmospheres 2 gas, maintained at 60°C for 3 hours. The water and excess sec-butylamine were distilled off, 50 ml of methanol was added, and 5.6 g of by-product potassium carbonate was obtained by filtration while hot, and the filtrate was evaporated and concentrated to obtain 9.63 g of the product sec-butylurea, with a one-pass conversion rate of 83.0%.

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Abstract

The invention discloses a method for synthesizing the secondary butyl urea adopting catalytic processes of carbon dioxide. It includes the following steps: preparing aqueous solution by potassium cyanate dissolved by water; putting the secondary butyl amine into the reactor and diluting them by water; adding the potassium cyanate solution into the secondary butyl amine and intimately mixing them; drumming gas of carbon dioxide to the said solution and reacting; distilling the water and the excess econdary butyl amine; filtering while the system is in a high temperature to obtain the by-product of potasium carbonate; decompressing and concentrating to the mixture to remove the alcohols and obtaining the product of secondary butyl urea. The invention is of low cost, simple method, cheap stock, and higher market value of by-product of potasium carbonate. The invention is extensively used in synthesizing the secondary butyl urea of chemical intermediate and is of broad market outlook.

Description

1. Technical field [0001] The invention relates to a method for synthesizing sec-butylurea, specifically a method using CO 2 A method for synthesizing sec-butylurea by catalytic method. 2. Background technology [0002] Herbicide is a major herbicide, and sec-butadiamide is one of the important raw materials for producing herbicide. At present, there is no relevant report on the synthesis of sec-butyl urea in China, and it has been produced by sulfuric acid catalysis abroad, that is, potassium cyanate aqueous solution and sec-butylamine are used to synthesize sec-butyl urea under the catalysis of 35% sulfuric acid, and the yield has reached 95%. %, but in the actual production process, the market value of the by-product potassium sulfate obtained by this method is not high, causing the cost of this method to be too high. 3. Contents of the invention [0003] The purpose of the present invention is to provide a CO 2 A method for synthesizing sec-butylurea by catalytic me...

Claims

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Application Information

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IPC IPC(8): C07C275/06C07C273/18
CPCY02P20/141
Inventor 范晓泉芮必胜严丽冉李春元
Owner NANJING UNIV
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