Isothermal differential reaction analyzer of mini-type gas-phase, liquid-phase and solid-phase slurry reactor

A differential reaction and micro-reactor technology, applied in analytical materials, chemical method analysis, instruments, etc., can solve the problems of difficulty in measuring reaction kinetic parameters of fast reactions, low reaction temperature, etc., and achieve mass transfer performance, fast, efficient, and economical. Space, the effect of preventing particle overflow

Inactive Publication Date: 2015-11-04
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to accurately measure the reaction rate, Xu Guangwen and others from the Institute of Process Engineering, Chinese Academy of Sciences developed a gas-solid reaction kinetic parameter instrument (CN200610171515.3), which uses a fluidized bed reactor, and the fluidized bed reactor can truly simulate and reproduce the actual solid material The gas-solid reaction and the corresponding heat transfer, mass transfer and diffusion process in the reactor have the best reliability and practicability, and the gas-solid reaction kinetic parameter instrument using this reactor is helpful to analyze the reaction Speed, reaction time, and comprehensive analysis of reaction kinetic parameters such as reaction activation energy to make up for the shortcomings of thermogravimetric analysis, but this kind of gas-solid reaction kinetic parameter instrument is especially suitable for applications that require online solid reactants to be added and the key product is gas. Gas-solid reaction, it is helpless for gas-liquid-solid three-phase reaction or gas-liquid reaction and the key product is liquid
As the most important fluidized bed reactor for the analyzer, the existing gas-liquid-solid three-phase reactor is usually not a real differential reactor, and there is no supporting good gas preheating device, resulting in a lower gas than the reaction temperature. The gas mixing, diffusion, reaction and other processes existing in this type of reactor will inevitably bring great difficulties to the measurement of the reaction kinetic parameters of the fast reaction

Method used

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  • Isothermal differential reaction analyzer of mini-type gas-phase, liquid-phase and solid-phase slurry reactor

Examples

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Effect test

Embodiment 1

[0031] Implementation example 1: Methyl methacrylate preparation experiment, feed nitrogen, take 25mL methanol and methacrolein mixed reaction solution, add 5% solid catalyst, when the temperature reaches 80°C and the pressure is 0.3Mpa, control and switch to feed oxygen , the gas flow rate is 200mL / min, and the test is carried out to obtain the in-situ infrared data of the concentration change of the functional group ester bond with time, which is increasing continuously, and the reaction rate at this temperature is confirmed, and the reaction kinetic model is further calculated according to the Arrhenus equation is = 0.792e 0.637t .

Embodiment 2

[0032]Implementation example 2: 2-methyl-2,4-pentanediol preparation experiment, pass nitrogen, take 25mL diacetone alcohol reaction liquid, add 5% nickel solid catalyst, when the temperature reaches 120 ° C, when the pressure is 1.5Mpa, control Switch to hydrogen gas, the gas flow rate is 200mL / min, and conduct a test to obtain the concentration change of the functional group ketone bond with time in the in-situ infrared data, which is continuously decreasing, and confirm the reaction speed at this temperature, and further calculate according to the Arrhenus equation The reaction kinetic model is = 0.458e -0.326t .

Embodiment 3

[0033] Implementation example 3: Terephthalic acid preparation experiment, blowing nitrogen gas, taking 25mL of p-xylene and acetic acid mixed reaction solution, adding 5% Co-Mn-Br solid catalyst, when the temperature reaches 200 °C and the pressure is 1.2Mpa, control switching Oxygen is introduced, the gas flow rate is 200mL / min, and the test is carried out to obtain the concentration change of the acid bond of the functional group with time in the in-situ infrared data, which is continuously increasing, and the reaction speed at this temperature is confirmed, and the reaction is further calculated according to the Arrhenus equation The kinetic model is = 0.0242e -6.8 / t .

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Abstract

The invention discloses an isothermal differential reaction analyzer of a mini-type gas-phase, liquid-phase and solid-phase slurry reactor. The isothermal differential reaction analyzer of the mini-type gas-phase, liquid-phase and solid-phase slurry reactor is applicable to monitoring and analysis of mini-type gas-phase, liquid-phase and solid-phase reactions. The isothermal differential reaction analyzer comprises a heating furnace provided with a thermoelectric couple, a gas pre-heating pipe and a gas buffering bottle connected with the gas pre-heating pipe, a mini-type reactor with a gas distributor and a multilayered ladder sand plate, and a condensation device and a gas filtering device which are connected with an outlet of the reactor in sequence, wherein the reactor is provided with an in-situ infrared device and a temperature control device; and a computer is used for switching introduced gas through a solenoid valve and carrying out flow control, and analyzing in-situ infrared and gas detection data. By virtue of the isothermal differential reaction analyzer disclosed by the invention, the mini-type slurry reactor is used for controlling reaction starting time in a real-time gas switching manner; and reaction changes can be relatively accurately monitored relative to liquid-phase and gas-phase monitoring results, so that analysis of catalyst inactivation reasons, reaction kinetic parameters and the like is relatively accurate.

Description

technical field [0001] The invention discloses a miniature gas-liquid-solid three-phase slurry bed isothermal differential reaction analyzer, belonging to the technical field of chemical analysis and testing. The miniature gas-liquid-solid three-phase slurry bed isothermal differential reaction analyzer can accurately control the reaction start time and reaction process, and determine the reaction kinetic parameters and catalyst deactivation reasons through comprehensive analysis. It is especially suitable for online gas phase switching, mixing and The liquid phase composition is monitored in real time and the key product is a gas-liquid-solid three-phase reaction in the liquid phase. Background technique [0002] Kinetic parameters of chemical reaction are important data for exploring the reaction mechanism, including chemical reaction rate, as well as various internal and external factors that affect the reaction rate during the reaction process (reaction substance structu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N35/00G01N31/00
Inventor 吕兴梅
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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