Method for preparing tetrapropylammonium bromide and horizontal autoclave

A technology of tetrapropylammonium bromide and horizontal reaction kettle, which is applied in the preparation of amino compounds from amines, organic chemistry, etc., can solve the problems affecting the synthesis of high-quality TS-1, the fluctuation of temperature, and the difficulty of reaction control, etc. The problem is that the reaction temperature is easy to control, the temperature distribution is uniform, and the Na+ content is low.

Inactive Publication Date: 2008-03-26
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Nevertheless, at the end of the reaction, the fluctuation range of temperature is still large, the difficulty of reaction control increases, and the quality of the product decreases, which affects the synthesis of high-quality TS-1
Therefore, it is very difficult to completely avoid the influence of solid products on the heat transfer in the reactor by increasing the stirring speed in the vertical reactor, and then improve the quality of TPAOH, and the energy consumption required for high speed is also very high

Method used

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  • Method for preparing tetrapropylammonium bromide and horizontal autoclave
  • Method for preparing tetrapropylammonium bromide and horizontal autoclave

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Embodiment 1

[0030] As shown in Figure 1, the horizontal reactor is a stainless steel pressure reactor, which includes: a kettle body 1, which is provided with a material inlet 11 and a discharge port 12; a jacket 2, which is arranged outside the kettle body 1 , with an inlet 21 and an outlet 22, used for heat removal in the reactor heating and reaction process, when heating or cooling, heating steam or cooling water enters from the jacket inlet 21 and comes out from the jacket outlet 22; and the agitator, the The stirrer includes a stirring motor 5 as a driving device, an axial stirring shaft 4 arranged in the kettle body 1 and driven by the stirring motor 5, and a total of 3 groups of radial shafts fixed on the stirring shaft 4 Stirring paddles 3, each set of stirring paddles 3 has paddle blades 31; the horizontal reactor is also provided with a pressure gauge 6 and a thermocouple 7 inside the tank body 1. The stirring paddle is selected from a deformed turbine paddle, and the ratio (a'b...

Embodiment 2

[0033] The aspect ratio of the horizontal reactor body is 1.8, the ratio of the diameter of the deformed turbine blade to the inner diameter of the reactor is 0.7, the ratio of the axial width of the blade to the length of the reactor is 0.22, the number of blades is 8, and the number of stirring blade groups Be 2, the rest are the same as embodiment 1.

[0034] Add bromopropane 730ml, about 8.03mol, and tri-n-propylamine 1270ml, about 6.72mol, into the above-mentioned 4L horizontal reactor at room temperature, and the molar ratio of the two substances is 1.2. The liquid content of the reactor was 0.6, stirring was started at a rotation speed of 100 rpm, and then the temperature was raised to 170° C. for 12 hours of reaction. After the reaction was over, the stirring was stopped and the temperature was lowered. The resulting solid product TPABr was collected by Buchner funnel filtration, and the filter cake was washed with ethyl acetate and dried in vacuo to obtain a solid pr...

Embodiment 3

[0036] The length-to-diameter ratio of the horizontal reactor body is 1.7, the ratio of the diameter of the deformed turbine blade to the inner diameter of the reactor is 0.6, the ratio of the axial width of the blade to the length of the reactor is 0.25, and the number of stirring blades is 6. Number of groups is 3, all the other with embodiment 1.

[0037] Add bromopropane 34.5L, about 379.7mol, and tri-n-propylamine 65.4L, about 346.2mol, into the above-mentioned 100L horizontal reactor at room temperature, and the molar ratio of the two substances is 1.1. The liquid content of the reactor was 0.55, and stirring was started at a rotation speed of 45 rpm, and then the temperature was raised to 150° C. for 12 hours of reaction. After the reaction was over, the stirring was stopped and the temperature was lowered. The resulting solid product TPABr was collected by Buchner funnel filtration, and the filter cake was washed with ethyl acetate and dried in vacuo to obtain a solid...

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Abstract

The present invention discloses process of preparing ammonium tetrapropyl bromide and the horizontal reaction kettle therefor. Through reaction of liquid 1-bromopropane and liquid n-tripropyl amine in a horizontal reaction kettle to obtain solid ammonium tetrapropyl bromide, filtering after reaction, washing the filter cake with organic solvent and drying, ammonium tetrapropyl bromide product with Na+ ion content lower than 0.1 ppm is prepared. Adopting horizontal reaction kettle for preparing ammonium tetrapropyl bromide has operation convenience, easy dispersion of both liquid phase and solid phase, favor to heat transfer, low energy consumption, improved reaction procedure, high yield and high product quality.

Description

technical field [0001] The invention relates to the field of preparation of tetrapropylammonium bromide, in particular to a method for preparing tetrapropylammonium bromide by reacting 1-bromopropane and tri-n-propylamine and the reaction kettle used, especially a horizontal reaction kettle. Background technique [0002] Titanium-silicon molecular sieve TS-1 is a highly efficient selective oxidation catalyst, which has the shape-selective effect of zeolite molecular sieve and H 2 o 2 With unique adsorption and activation properties, it can be used for selective catalytic oxidation of various organic substances, in the epoxidation of olefins, the hydroxylation of benzene and phenol (A.Thangaraj, R.Kumar, P.Ratnasamy, et al.Catalytic Properties of Crystalline Titanium Silicalites.II.Hydroxylation of Phenol with Hydrogen Peroxide over TS-1Zeolites[J].Journal of Catalysis.1991,131:294-297), oximation of cyclohexanone (A.Thangaraj, S.Sivasanker, P .Ratnasamy.Catalytic Properti...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/68
Inventor 曹贵平张明华白伟民张大伟
Owner EAST CHINA UNIV OF SCI & TECH
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