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Continuous synthesis process and device for 3-bromopyridine

A technology for chemical synthesis and bromopyridine, which is applied in the field of 3-bromopyridine continuous synthesis process and equipment, can solve the problems of complex post-treatment, low reaction efficiency, and long intermittent reaction time of 3-bromopyridine, and achieve simplified reaction post-processing , Promote complete liquid separation, shorten the effect of neutralization liquid separation time

Inactive Publication Date: 2020-12-25
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a 3-bromopyridine continuous synthesis process and device, which can effectively solve the problems existing in the synthesis of 3-bromopyridine, improve production efficiency, reduce energy consumption, save production costs, and can solve the problem of 3-bromopyridine synthesis. The problems of long batch reaction time, complicated post-treatment and low reaction efficiency

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  • Continuous synthesis process and device for 3-bromopyridine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Such as figure 1 , a 3-bromopyridine continuous synthesis device, including a mixer 1, a first-stage tubular reactor 2, a second-stage tubular reactor 3, a first condenser 4, a continuous neutralization and liquid separation device 5, and a waste water storage tank 6 , negative pressure film evaporator 7, second condenser 8, negative pressure rectification tower 9, third condenser 10, product storage tank 11, reboiler 12, rectification bottom material storage tank 13, pyridine, hydrobromic acid After being metered by the metering pump, hydrogen peroxide and hydrogen peroxide are respectively connected to the three liquid inlets of the mixer 1, the liquid outlet of the mixer 1 is connected to the liquid inlet of the first-stage tubular reactor 2, and the liquid outlet of the first-stage tubular reactor 2 is connected to the second-stage pipe Type reactor 3 liquid inlet, the first-stage tubular reactor 2 is heated by steam condensed water, the second-stage tubular reactor...

Embodiment 2

[0034] The steps of 3-bromopyridine continuous synthesis technique are as follows:

[0035] Pyridine, hydrobromic acid and hydrogen peroxide are injected into the mixer 1 respectively in a molar ratio (1:4:1), the concentration of hydrobromic acid is 48%, and the concentration of hydrogen peroxide is 50%. After being mixed in the mixer 1, it enters the first-stage tubular reactor 2 for reaction. , the reaction temperature is 50°C, the residence time is 5min, the reaction liquid enters the second-stage tubular reactor 3 to continue the reaction, the reaction temperature is 90°C, the residence time is 20min, the reacted reaction liquid enters the first condenser 4 and is cooled to 10°C, after cooling The reaction liquid enters the continuous neutralization and liquid separation device 5, and 30% liquid caustic soda is added simultaneously and enters the continuous neutralization liquid separation device 5, the upper layer water phase enters the waste water storage tank 6, and the...

Embodiment 3

[0037] The steps of 3-bromopyridine continuous synthesis technique are as follows:

[0038] Pyridine, hydrobromic acid and hydrogen peroxide are injected into the mixer 1 respectively in a molar ratio (1:4:1.2), the concentration of hydrobromic acid is 49%, and the concentration of hydrogen peroxide is 50%. After being mixed in the mixer 1, it enters the first-stage tubular reactor 2 for reaction , the reaction temperature is 50°C, the residence time is 5min, the reaction liquid enters the second-stage tubular reactor 3 to continue the reaction, the reaction temperature is 90°C, the residence time is 20min, the reacted reaction liquid enters the first condenser 4 and is cooled to 10°C, after cooling The reaction liquid enters the continuous neutralization and liquid separation device 5, and 30% liquid caustic soda is added simultaneously and enters the continuous neutralization liquid separation device 5, the upper layer water phase enters the waste water storage tank 6, and th...

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Abstract

The invention discloses a continuous synthesis process and device of 3bromopyridine, which comprises the following steps: respectively pumping pyridine, hydrobromic acid and hydrogen peroxide into a mixer according to a certain proportion, mixing by the mixer, and reacting in a first-stage tubular reactor and a second-stage tubular reactor; a reaction solution obtained after the reaction of the first-section tubular reactor and the second-section tubular reactor enters a first condenser to be cooled, the cooled reaction solution enters a continuous neutralization and liquid separation device,and meanwhile a sodium hydroxide solution is added into the continuous neutralization and liquid separation device; an upper-layer water phase of the continuous neutralization liquid separation deviceenters a wastewater storage tank, a lower-layer organic phase is evaporated and flashed by a negative-pressure film evaporator to remove low-boiling-point substances brought by separated liquid and then enters a negative-pressure rectifying tower to be rectified, the reflux ratio is controlled, a product at the top of the negative-pressure rectifying tower is collected by a product storage tank,and a bottom material at the bottom of the negative-pressure rectifying tower can be used as high-calorific-value fuel. The method can effectively solve the problems in 3bromopyridine synthesis, improves the production efficiency, reduces the energy consumption, and saves the production cost.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a 3-bromopyridine continuous synthesis process and device. Background technique [0002] 3-Bromopyridine, also known as m-bromopyridine, molecular formula C 5 h 4 BrN, molecular weight 158, colorless to light yellow liquid or light brown liquid, relative density 1.64g / mL (relative to water), boiling point 173°C (atmospheric pressure). Soluble in water, ethanol and ether, the solubility in water is 31g / L (20°C). [0003] As an important organic synthesis intermediate, 3-bromopyridine is widely used in the field of medicine. It is an important raw material and intermediate for the antidepressant zimetidine hydrochloride, the neurological drug propacramer, and the prostate cancer drug abiraterone , can also be used in the synthesis of 3-methylaminopiperidine, an intermediate of baloxacin, a medicine of the class of sandacins; in addition, 3-bromopyridine is also used in...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61Y02P20/10
Inventor 方红新温兰兰李凯赵德张刘彬
Owner ANHUI COSTAR BIOCHEM CO LTD
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