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2-vinylpyridine reaction post-treatment method and device

A technology of vinylpyridine and reaction, applied in the field of 2-vinylpyridine post-reaction treatment method and its device, can solve the problems of long static stratification time, large amount of liquid caustic soda, etc., to speed up extraction and stratification, improve production Efficiency, reducing the effect of layering and standing time

Inactive Publication Date: 2020-12-29
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a 2-vinylpyridine post-reaction treatment method and its device, which can effectively solve the problems existing in the dehydration reaction post-treatment, improve production efficiency, reduce energy consumption, save production costs, and can solve the problem of 2-vinylpyridine reaction post-treatment. The problem of large amount of liquid caustic soda used in pyridine dehydration reaction and long standing time for stratification

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  • 2-vinylpyridine reaction post-treatment method and device

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Comparison scheme
Effect test

Embodiment 1

[0025] refer to figure 1 , a 2-vinylpyridine reaction post-processing device, comprising a dehydration reactor 1, a first condenser 2, a second condenser 3, a pump A4, an extraction kettle 5, a liquid separation mirror 6, an aqueous storage tank 7, Distillation kettle 8, third condenser 9, solvent storage tank 10, vacuum kettle 11, fourth condenser 12, pump B13, four-way regulating valve 14, 2-vinylpyridine storage tank 15, bottom material tank 16, dehydration The gas phase outlet of reaction kettle 1 is connected to the inlet of first condenser 2, the liquid outlet of first condenser 2 is connected to the inlet of second condenser 3, and the first condenser 2 and second condenser 3 are connected in series to synthesize The liquid is cooled step by step. The refrigerant of the first condenser 2 is cooled by circulating water, and the waste heat of the circulating water is used to directly heat and recover the solvent as the heat source of the still 8. The refrigerant of the se...

Embodiment 2

[0028] The mixture of 2-vinylpyridine and water evaporated from the dehydration reactor 1 under reduced pressure passes through the first condenser 2 at an outlet temperature of 60°C, and after being cooled by the second condenser 3, the outlet temperature of the liquid is 5°C, and then enters the extraction kettle 5 , add 3 times the extraction solvent dichloromethane of distilled liquid volume, leave standstill 30min layering after stirring for 5min, the upper layer water phase introduces water phase storage tank 7, the lower floor organic phase introduces distillation kettle 8 to reclaim dichloromethane, distillation kettle 8 gas phase The temperature is 60°C, the evaporated phase is condensed by the third condenser 9 and then introduced into the solvent storage tank 10, the distillation bottom liquid is introduced into the vacuum kettle 11, and 2-vinylpyridine is evaporated under reduced pressure, and collected at 70-100°C / 30-100mm / The Hg colorless and transparent fraction...

Embodiment 3

[0030]The mixed solution of 2-vinylpyridine and water evaporated from the dehydration reactor 1 under reduced pressure passes through the first condenser 2 at an outlet temperature of 60°C, and after being cooled by the second condenser 3, the outlet temperature of the liquid is 10°C, and then enters the extraction kettle 5 , add 2 times the extraction solvent dichloromethane of distilled liquid volume, after stirring for 20min, let stand for 50min to separate layers, the upper layer water phase is introduced into the water phase storage tank 7, and the lower organic phase is introduced into the still 8 to reclaim the dichloromethane, and the still 8 gas phase The temperature is 50°C, the evaporated phase is condensed by the third condenser 9 and introduced into the solvent storage tank 10, the bottom liquid of the distillation is introduced into the vacuum kettle 11, and 2-vinylpyridine is evaporated under reduced pressure, and collected at 70-100°C / 30-100mm / The Hg colorless ...

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Abstract

The invention discloses a 2-vinylpyridine reaction post-treatment method and device, and the method comprises the steps: 1, carrying out the two-stage cooling of a mixed solution of 2-vinylpyridine distilled from a dehydration reaction kettle under reduced pressure and water through a first condenser and a second condenser, pumping the cooled mixed solution into an extraction kettle, adding an extraction solvent, uniformly stirring, standing, and layering; 2, introducing an upper-layer water phase of the extraction kettle into a water phase storage tank, and introducing a lower-layer organic phase into a distillation kettle to recover dichloromethane; and 3, condensing the evaporated phase by a third condenser, introducing the condensed evaporated phase into a solvent storage tank, introducing the distillation base solution into a reduced pressure kettle, carrying out reduced pressure distillation to obtain 2-vinylpyridine, returning the fraction before distillation to the distillationkettle, continuously purifying, distilling the middle-section fraction to obtain the finished 2-vinylpyridine, and taking the distillation base material as the incinerator fuel. The method provided by the invention can effectively solve the problems of dehydration reaction post-treatment, improves the production efficiency, reduces the energy consumption, saves the production cost, and solves theproblems of large use amount of liquid caustic soda and long standing layering time in the 2-vinylpyridine dehydration reaction.

Description

technical field [0001] The invention relates to the technical field of chemical reaction post-treatment, in particular to a 2-vinylpyridine post-reaction treatment method and a device thereof. Background technique [0002] 2-Vinylpyridine is a widely used intermediate in organic synthesis. It can form terpolymer latex with butadiene and styrene. It is the skeleton material of rubber products such as tires and conveyor belts. my country's annual demand is tens of thousands tons and increasing year by year. In addition, 2-vinylpyridine, as an important polymer monomer, also has important applications in medicine, ion exchange resins and chemical films. [0003] The synthesis methods of 2-vinylpyridine mainly include one-step method and two-step method: gas-phase one-step method, less reaction process steps, gas-solid catalytic reaction, using fixed bed reactor for synthesis, simple operation, but the reaction temperature needs to be above 300°C, and 2-Vinylpyridine is easy to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/16C07D213/127
CPCC07D213/16
Inventor 温兰兰吴李瑞孔军军赵来红刘彬
Owner ANHUI COSTAR BIOCHEM CO LTD