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Method for preparing tetrabutylurea by oil-water two-phase reaction system

A tetrabutylurea, phase reaction technology, applied in the preparation of urea derivatives, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor reaction selectivity, slow reaction rate, poor water solubility, etc. Effects of corrosion, reduced process cost, improved conversion and product selectivity

Inactive Publication Date: 2021-08-17
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Considering the severe toxicity of reaction raw material phosgene, the Chinese patent that publication number is CN105837473A discloses a kind of use bis(trichloromethyl)carbonate (bis(trichloromethyl)carbonate) to replace phosgene, bis( Trichloromethyl)carbonate is crushed and mixed with an aqueous solution of a strong base. After fully stirring, dibutylamine is added dropwise to react, which basically realizes the nontoxic and harmless reaction raw materials, but bis(trichloromethyl)carbonate is water-soluble Poor performance, the reaction interface is liquid-solid reaction, the reaction rate is slow
Publication number is that the Chinese patent of CN106478461A discloses a kind of with ethanol instead of water as solvent, to solve the problem of bis(trichloromethyl)carbonate water solubility is not good, bis(trichloromethyl)carbonate is dissolved in ethanol , slowly drop into dibutylamine through a constant pressure funnel, which improves the reaction rate, but the reaction selectivity is poor and the yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 1.68 grams of bis(trichloromethyl)carbonate, dissolve it in 31.68 grams of dichloroethane, add it to a 250 mL three-necked flask, measure 30 mL of deionized water, and add it to the three-necked flask as a liquid seal Weigh 27.43 grams of dibutylamine, dissolve in 15.02 grams of dichloroethane, place in a 50 mL micro-injection pump, set the injection rate of the micro-injection pump to 9 mL / h, and start stirring, and the reaction temperature is controlled at 45 ° C. After the feeding is completed, the reaction is continued after sealing the reactor, wherein the feeding time is about 5 hours, and the reaction residence time is about 3 hours. After the reaction is finished, the reaction liquid is separated with a separatory funnel, the organic phase is washed with water and distilled under reduced pressure to obtain a crude product of tetrabutylurea, and the crude product is distilled under reduced pressure to obtain a product of tetrabutylurea. At the same time, th...

Embodiment 2

[0018] Weigh 1.62 grams of bis(trichloromethyl)carbonate, dissolve it in 32.38 grams of dichloroethane, add it to a 250 mL three-necked flask, measure about 30 mL of deionized water, and add it to the three-necked flask as a solution. Seal; Weigh 16.9 grams of dibutylamine, dissolve in 25 grams of dichloroethane, place in a 50 mL micro-injection pump, set the injection rate of the micro-injection pump to 9 mL / h, start stirring, and control the reaction temperature at 45 °C , After the feeding is completed, the closed reactor continues to react, wherein the feeding time is about 5h, and the reaction residence time is about 3h. After the reaction is finished, the reaction liquid is separated with a separatory funnel, the organic phase is washed with water and distilled under reduced pressure to obtain a crude product of tetrabutylurea, and the crude product is distilled under reduced pressure to obtain a product of tetrabutylurea. Simultaneously, the unreacted dibutylamine can b...

Embodiment 3

[0020] Weigh 1.66 grams of bis(trichloromethyl)carbonate, dissolve it in 35.80 grams of cyclohexane, add it to a 250 mL three-necked flask, measure 30 mL of deionized water, and also add it to a three-necked flask; weigh dibutylamine 16.91 grams, dissolved in 10 grams of cyclohexane, placed in a 50 mL micro-injection pump, the injection rate of the micro-injection pump was set at 3 mL / h, and stirring was started, and the reaction temperature was controlled at about 35 °C. The reaction feed time is about 8 hours. After the reaction is over, the reaction liquid is separated with a separatory funnel, and the organic phase is washed with water and refined by vacuum distillation to obtain the crude product of tetrabutylurea. The crude product can be obtained by vacuum distillation Tetrabutylurea products. Simultaneously, the unreacted dibutylamine can be recycled through recovery, and it can be obtained through analysis that the conversion rate of bis(trichloromethyl)carbonate can ...

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Abstract

The invention discloses a method for preparing tetrabutylurea by using an oil-water two-phase reaction system, which is characterized in that bis (trichloromethyl) carbonate and dibutylamine are used as raw materials, the oil-water two-phase reaction system is designed and provided, a solvent capable of effectively dissolving bis (trichloromethyl) carbonate and dibutylamine is adopted, meanwhile, a water phase is added into the reaction system to perform liquid seal on the reaction system, can absorb hydrogen chloride gas generated by the reaction at the same time, and promotes the forward proceeding of the whole reaction, and the method has the characteristics of high conversion rate, high selectivity and the like. The method for preparing tetrabutylurea by using the oil-water two-phase reaction system comprises the following steps: dissolving bis (trichloromethyl) carbonate in an organic solvent, placing the solution in a reactor, and simultaneously adding water into the reactor to perform liquid seal on the reaction system; and dissolving dibutylamine in an organic solvent, slowly injecting the dibutylamine into the organic solution of bis (trichloromethyl) carbonate through a micro-injection pump, carrying out chemical reaction, and carrying out refining treatment to obtain the product tetrabutylurea.

Description

technical field [0001] The invention relates to a method for preparing high-purity tetrabutylurea, more specifically to a method for preparing tetrabutylurea in an oil-water two-phase reaction system. Background technique [0002] Tetrabutylurea (1,1,3,3-Tetrabutylurea, CAS 4559-86-8) is a transparent or slightly yellowish liquid with a relative density of 0.887 at 25°C and a melting point of -51°C / 760mm Hg , the flash point is 93°C, the boiling point is 379.8°C / 760mmHg, the viscosity is slightly larger than water, the solubility is similar to that of tetramethylurea, and it is miscible with most organic reagents such as petroleum ether, etc. It is a widely used It can also be used as a solvent, extractant and catalyst for organic synthesis. In addition, because the solubility of hydrogenated anthraquinone in tetrabutyl urea is greater than that of trioctyl phosphate, the hydrogenation efficiency in the hydrogen peroxide production process is improved, and the distribution ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/06
CPCC07C273/1809C07C273/189C07C275/06
Inventor 刘定华居海军崔德文郭春花万建龙刘晓勤
Owner NANJING UNIV OF TECH
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