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Method for preparing high-purity tetrapropylammonium bromide

A tetrapropylammonium bromide, high-purity technology, applied in the field of tetrapropylammonium bromide preparation, can solve the problems of low purity of tetrapropylammonium bromide, many impurities, etc., achieve good use prospects and high purity of finished products Effect

Inactive Publication Date: 2019-04-19
JIANGXI KENTE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Though the existing method for preparing tetrapropyl ammonium bromide can produce tetrapropyl ammonium bromide, as the patent of CN102020570A as notification number, the tetrapropyl ammonium bromide purity of preparation is not high, and impurity is more, and people are in Also need to remove impurities to use during use, and this has just brought inconvenience to the user

Method used

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  • Method for preparing high-purity tetrapropylammonium bromide
  • Method for preparing high-purity tetrapropylammonium bromide

Examples

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Effect test

Embodiment 1

[0022] A method for preparing high-purity tetrapropylammonium bromide, the concrete steps are as follows:

[0023] Step 1, mix tri-n-propylamine, 1-bromopropane and butanone in an autoclave, the molar ratio of tri-n-propylamine and 1-bromopropane is 1:1.1, the temperature of the autoclave is 145 degrees Celsius, and the pressure is 0.68MPa, The temperature rise reaction is carried out under stirring. The system after the reaction is a solid-liquid two-phase, the solid phase is tetrapropylammonium bromide, and the liquid phase is unreacted raw materials. After the reaction is completed, an appropriate amount of water is added thereto, and the solid phase is dissolved in water to obtain Tetrapropylammonium bromide aqueous solution, tetrapropylammonium bromide aqueous solution is immiscible with unreacted raw material, separates and obtains tetrapropylammonium bromide aqueous solution;

[0024] Step 2: Distill the tetrapropylammonium bromide aqueous solution under reduced pressur...

Embodiment 2

[0028] A method for preparing high-purity tetrapropylammonium bromide, the concrete steps are as follows:

[0029] Step 1, mix tri-n-propylamine, 1-bromopropane and ethyl acetate in an autoclave, the molar ratio of tri-n-propylamine and 1-bromopropane is 1:1.2, heat up reaction under stirring, the system after reaction is solid Two phases of liquid, the solid phase is tetrapropylammonium bromide, the liquid phase is unreacted raw materials, after the reaction is completed, add an appropriate amount of water to it, and the solid phase is dissolved in water to obtain tetrapropylammonium bromide aqueous solution, tetrapropylammonium bromide Aqueous solution of ammonium chloride is immiscible with unreacted raw material, separates and obtains aqueous solution of tetrapropylammonium bromide;

[0030] Step 2, the tetrapropylammonium bromide aqueous solution is distilled under reduced pressure to recover ethyl acetate, and then the remaining products are dried to obtain the tetraprop...

Embodiment 3

[0034] A method for preparing high-purity tetrapropylammonium bromide, the concrete steps are as follows:

[0035] Step 1, mix tri-n-propylamine, 1-bromopropane and acetone in an autoclave, the molar ratio of tri-n-propylamine and 1-bromopropane is 1:1.3, the temperature of the autoclave is 152 degrees Celsius, the pressure is 0.65MPa, stir The temperature rise reaction is carried out under the following conditions. The system after the reaction is a solid-liquid two-phase, the solid phase is tetrapropylammonium bromide, and the liquid phase is unreacted raw materials. Propyl ammonium bromide aqueous solution, tetrapropyl ammonium bromide aqueous solution is immiscible with unreacted raw material, separates and obtains tetrapropyl ammonium bromide aqueous solution;

[0036] In step 2, tetrapropylammonium bromide aqueous solution is distilled under reduced pressure to recover acetone, and then the remaining products are dried, and rinsed with a modifier for 2 minutes. The modif...

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Abstract

The invention discloses a method for preparing high-purity tetrapropylammonium bromide. The method concretely comprises the following steps: 1, mixing tri-n-propylamine, 1-bromopropane and a solvent in an autoclave, heating and reacting the obtained mixture under a stirring condition, adding an appropriate amount of water after the reaction, and performing separation to obtain an aqueous solutionof tetrapropylammonium bromide; 2, carrying out reduced pressure distillation and drying on the aqueous solution of tetrapropylammonium bromide to obtain crude tetrapropylammonium bromide; 3, dissolving the crude tetrapropylammonium bromide in isopropyl alcohol, adding a sodium hydroxide solution, performing ultrasonic uniform mixing, and then treating the obtained solution in a magnetic field toobtain a first mixed solution; and 4, adding a hydrobromic acid solution to the first mixed solution, heating and refluxing the obtained solution, performing heat insulation to obtain a second mixed solution, cooling the second mixed solution to achieve crystallization, filtering the cooled solution, and carrying out reduced pressure distillation on the obtained product to obtain the tetrapropylammonium bromide. The finished tetrapropylammonium bromide prepared in the invention has a high purity and a good use prospects.

Description

technical field [0001] The invention relates to the field of preparation of tetrapropylammonium bromide, in particular to a method for preparing high-purity tetrapropylammonium bromide. Background technique [0002] A catalyst is a substance that can change the chemical reaction rate (increase or decrease) of the reactants in a chemical reaction without changing the chemical balance, and its own quality and chemical properties have not changed before and after the chemical reaction. Catalysts are used in more than 90% of industrial processes, such as chemical, petrochemical, biochemical, and environmental protection. Catalysts play an extremely important role in the modern chemical industry. For example, iron catalysts are used in the production of synthetic ammonia, vanadium catalysts are used in the production of sulfuric acid, and different catalysts are used in the production of three major synthetic materials such as the polymerization of ethylene and the use of butadie...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/12C07C209/84
CPCC07C209/12C07C209/84C07C211/63
Inventor 刘鸿王志军吴小建
Owner JIANGXI KENTE CHEM CO LTD
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