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Method for synthesizing sec-butyl urea

A technology of sec-butylurea and sec-butylamine, applied in the field of compound synthesis, can solve the problems of poor safety, inconvenient operation process and high product cost, and achieve the effects of simple production equipment requirements, low cost and easy operation.

Inactive Publication Date: 2007-05-02
NANJING AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Technical Problem The purpose of this invention is to provide a method for synthesizing sec-butylurea, which overcomes the defects of high product cost, poor safety, and inconvenient operation process in the prior art. The raw materials of this method are easy to obtain, and storage and transportation And the production process is safer

Method used

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  • Method for synthesizing sec-butyl urea
  • Method for synthesizing sec-butyl urea
  • Method for synthesizing sec-butyl urea

Examples

Experimental program
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Effect test

Embodiment 1

[0028] In a 250mL three-necked flask, add 70g of water, 0.5mol (36.5g) sec-butylamine, and 5 drops of methyl red ethanol solution, install a dropping funnel, a thermometer, and an electric stirrer, and place the three-necked flask in an ice-water bath . Add about 50g of 36-38% hydrochloric acid into the dropping funnel, start the electric stirrer, start dropping, control the dropping speed, make the temperature not exceed 20°C, stop dropping when the solution turns red, and stop stirring. Remove the ice-water bath and the dropping funnel, dry the surface of the three-necked bottle, add 1.5mol (90g) of urea, place the three-necked bottle in an electric heating bag, install a condenser tube, pass condensed water, start stirring, heat and reflux for 4 hours, stop heating, and wait for When the temperature drops below 80°C, pour the reaction liquid into a 250mL beaker under heat, and crystallize naturally for 0.5h, then place it in the refrigerator for crystallization for more tha...

Embodiment 2

[0030] In a 250mL three-necked flask, add 100g of water, 0.5mol (36.5g) sec-butylamine, and 5 drops of methyl red ethanol solution, install a dropping funnel, a thermometer, and an electric stirrer, and place the three-necked flask in an ice-water bath . Add about 49 g of concentrated sulfuric acid into the dropping funnel, start the electric stirrer, start dropping, control the dropping speed, make the temperature not exceed 20°C, stop dropping when the solution turns red, and stop stirring. Remove the ice-water bath and the dropping funnel, dry the surface of the three-necked bottle, add 1.5mol (90g) of urea, place the three-necked bottle in an electric heating bag, install a condenser tube, pass condensed water, start stirring, heat and reflux for 4 hours, stop heating, and wait for When the temperature drops below 80°C, pour the reaction liquid into a 250mL beaker under heat, and crystallize naturally for 0.5h, then place it in the refrigerator for crystallization for more...

Embodiment 3

[0032] On the 1000L enamel reaction kettle equipped with agitator, install condensing reflux device, temperature control device, freezing device, heating device, dripping device and pH value measuring device respectively. Add 280kg of water, 146kg of sec-butylamine, add 36-38% hydrochloric acid into the dripping device, start stirring, start the freezing device, start adding hydrochloric acid dropwise, control the dropping speed, so that the temperature does not exceed 20°C until the pH value reaches 5 At ~5.5 o'clock, stop dropping, stop stirring, and close the freezing device. Add 270 kg of urea, heat to reflux for 4 hours, stop heating, and crystallize naturally for 2 hours, then start the freezer, and crystallize at -1 ~ -5°C for more than 6 hours. The white solid was obtained by suction filtration, washed with 10 kg of cold water, drained, and weighed. Add water equivalent to 1.5 times the weight of the white solid, heat to dissolve, and crystallize naturally for 2 hours...

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Abstract

A process for synthesizing para-butyl urea from para-butyl amine, acid and urea through salting reaction in water, and reflux reaction. Its sewage can be used to prepare fertilizer.

Description

1. Technical field [0001] The invention relates to a production technology of sec-butylurea, belongs to the technical field of compound synthesis, and is specially used for synthesizing sec-butylurea. 2. Background technology [0002] S-butylurea is an important chemical raw material, which can be used to synthesize the herbicide bromacil (3-sec-butyl-5-bromo-6-methyluracil), and can also be used for the synthesis of medicine or other chemical products . [0003] Its synthetic method was first invented by John Kenson Simons et al. (US Patent, 2673859, 1954-03-30), and the reaction equation is: [0004] [0005] This method not only requires many types of raw materials, but also needs high temperature and high pressure to react, and the product cost is high, so it is not suitable for industrial production. At present, the enterprise uses the phosgene method to produce, and the reaction equation is: [0006] [0007] This method requires the use of highly toxic phosge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/06C07C273/18
Inventor 杨春龙
Owner NANJING AGRICULTURAL UNIVERSITY
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