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Method for preparing tert-n-propyl ammonium bromide

A technology of propylammonium bromide and tri-n-propylamine is applied in the field of preparation of tetra-n-propylammonium bromide, and can solve the problems of high TPABr yield, affecting reaction rate, reaction yield TPABr quality, low TPABr yield and the like , to achieve the effect of speeding up the reaction rate, easy engineering implementation, and uniform crystal particle size

Inactive Publication Date: 2018-12-21
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the low yield of TPABr existing in the prior art, and the coagulation of TPABr in the reactor affects the problems of reaction rate, reaction yield and quality of reaction product TPABr, the present invention proposes a preparation of tetra-n-propylammonium bromide Method, the TPABr yield obtained by the preparation method of the present invention is high (92%), has overcome the coagulation problem of reaction product TPABr, has improved the quality of reaction product TPABr, accelerated reaction rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 prepares TPABr without adding solvent

[0019] CH 3 CH 2 CH 2 Br+(C 3 h 7 ) 3 N=(CH 3 CH 2 CH 2 ) 4 NBr

[0020] According to the molar ratio n(1-bromopropane):n(tri-n-propylamine)=1.1:1, 13.53g (0.11mol) of 1-bromopropane and 14.33g of tri-n-propylamine were added to the polytetrafluoroethylene-lined stainless steel reactor (0.1mol), stir evenly, seal the reactor, and the pressure condition is autogenous pressure (in a container with equal volume, if the temperature changes, it will cause a change in pressure, which is the autogenous pressure), and the reactor is placed in In the oven, heat up to 100°C, start timing when the temperature is constant at 100°C, take out the reaction kettle after several hours of reaction (16, 18, 20, 22, 24h), use ethyl acetate to wash and suction filter the reaction product, and put The solid sample filtered by suction was put into a vacuum drying oven and dried until the mass was constant, weighed and calculated ...

Embodiment 2

[0024] Embodiment 2 adds different solvents and prepares TPABr

[0025] According to the molar ratio n (solvent):n (1-bromopropane):n (tri-n-propylamine)=5:1.1:1, solvent (add a kind of solvent at a time, solvent is respectively water, acetone, methyl alcohol, ethanol, acetic acid Ethyl ester, xylene), 1-bromopropane, and tri-n-propylamine were added to a polytetrafluoroethylene-lined stainless steel reactor, and the quality of the added tri-n-propylamine was 14.33g (0.1mol), and the quality of 1-bromopropane was 13.53g (0.11mol), stir evenly, seal the reaction kettle, the pressure condition is self-generated pressure, place the reaction kettle in an oven, heat up to 100°C, start timing when the temperature is constant at 100°C, and react for 14h. After the reaction is finished, the reaction solution is cooled, and then it is washed and suction-filtered with ethyl acetate (when the solvent is water, methanol, and ethanol, the solvent and 1-bromopropane are recovered by distill...

Embodiment 3

[0029] Embodiment 3 adds the ethanol solvent of different consumptions and prepares TPABr

[0030] According to the molar ratio n(ethanol):n(1-bromopropane):n(tri-n-propylamine)=(1~5):1.1:1, 4.61~23.04g (0.1~0.5mol) ethanol, 13.53g (0.11 mol) 1-bromopropane and 14.33g (0.1mol) tri-n-propylamine were added to a polytetrafluoroethylene-lined stainless steel reactor, stirred evenly, and the reactor was sealed. The reactor was placed in an oven and heated to 100°C. Start timing at a constant temperature of 100°C, and react for 14 hours under autogenous pressure. After the reaction, the reaction solution was distilled under reduced pressure to reclaim ethanol and excess 1-bromopropane. Then, ethyl acetate was added for washing and suction filtration, and the solid sample filtered by suction was put into a vacuum drying oven and dried until the quality was constant. Weigh and calculate the yield, and use the molar method to determine the mass fraction of the product. During the ex...

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PUM

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Abstract

The invention discloses a method for preparing tert-n-propyl ammonium bromide. The method comprises the following steps: by taking 1-bromopropane and tri-n-propylamine as raw materials and ethanol asa solvent, synthesizing tert-n-propyl ammonium bromide in a reaction kettle, wherein the ethanol, the 1-bromopropane and the tri-n-propylamine are added in a mole ratio of 2.8 to 1.1 to 1, and a reaction yield is as high as 92%. By adopting the method, ethanol which is small in toxicity is adopted as the solvent, the reaction velocity can be increased, and the prepared tert-n-propyl ammonium bromide is uniform in crystal granularity, high in purity, high in yield, simple in operation step, low in production cost and good in industrial application prospect.

Description

technical field [0001] The invention relates to the field of preparation of tetra-n-propylammonium bromide, in particular to a preparation method of tetra-n-propylammonium bromide. Background technique [0002] Tetra-n-propylammonium hydroxide (TPAOH) is the only alkali source and template agent for the synthesis of a new type of catalytic material - titanium silicon molecular sieve TS-1. At present, TS-1 molecular sieve has been realized in the process of phenol oxidation to hydroquinone It has been industrialized, and it also shows good industrial application prospects in important petrochemical processes such as the preparation of cyclohexanone oxime by the ammoxidation of cyclohexanone and the preparation of propylene oxide by the epoxidation of propylene. However, one of the important problems is that the cost is high. , The price and consumption of TPAOH are the main factors affecting the cost of molecular sieves. [0003] TPAOH is not available in China at present, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/12C07C211/63
CPCC07C209/12C07C211/63
Inventor 冯利利王东星王召滨王世伟
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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