The method provides a production process for preparing tetrabromoethane using a microchannel reactor, including the following steps:
(1) The raw material bromine is continuously introduced into the microchannel reactor driven by the power system;
(2) Acetylene is continuously introduced into the microchannel reactor through the gas mass flow controller;
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; Control the temperature of reactants through the heat exchange system;
(4) After the reaction process is completed, the products are collected through the gas-liquid separator; The collected products are added with stabilizer after passing the analysis, and then packaged into products.
The invention uses a microchannel reactor to prepare tetrabromoethane. The main equipment includes:
(1) Raw material and power system: (a) bromine raw material tank, (b) acetylene raw material tank;
(2) Heat exchange system;
(3) Reaction and heat exchange system;
(4) Finished products and filling system. The bromine raw material tank is a glass-lined tank; Acetylene raw material tank is acetylene cylinder; The microchannel reactor is made of glass, and the finished product tank is a glass-lined tank. Among them, the microchannel reactor in the reaction and heat exchange system is five microchannel glass reactors used in series.
Example 1:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 500 μ m； The total volume of the reaction zone of the microchannel reactor is 27 ml;
(2) The raw material bromine is continuously fed into the microchannel reactor at a flow rate of 0.7kg/min driven by the plunger pump of the power system; Acetylene is continuously introduced into the microchannel reactor through the gas mass flow controller at a flow rate of 0.057kg/min; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; The system pressure in the microchannel reactor is 0.2 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 4 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 98.7% and the yield is 98.2%.
Example 2:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 1000um; The total volume of reaction zone of microchannel reactor is 45ml;
(2) Under the drive of the plunger pump of the power system, the raw material bromine is continuously introduced into the microchannel reactor at a flow rate of 0.8kg/min; Acetylene is continuously introduced into the microchannel reactor through the gas mass flow controller at a flow rate of 0.065kg/min; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; The system pressure in the microchannel reactor is 0.3 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 6 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 98.6% and the yield is 98.4%.
Example 3:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 1500um; The total volume of the reaction zone of the microchannel reactor is 54 ml;
(2) Under the drive of the plunger pump of the power system, the raw material bromine is continuously introduced into the microchannel reactor at a flow rate of 0.9 kg/min; Acetylene is continuously introduced into the microchannel reactor through the gas mass flow controller at a flow rate of 0.073kg/min; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; The system pressure in the microchannel reactor is 0.4 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 8 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 98.5% and the yield is 98.3%.
Example 4:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 2000um; The total volume of the reaction zone of the microchannel reactor is 63ml;
(2) Under the drive of the plunger pump of the power system, the raw material bromine is continuously introduced into the microchannel reactor at a flow rate of 1.0kg/min; Acetylene is continuously introduced into the microchannel reactor at a flow rate of 0.08kg/min through the gas mass flow controller; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; The system pressure in the microchannel reactor is 0.5 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 10 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 98.5% and the yield is 98.3%.
Example 5:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 500um; The total volume of reaction zone of microchannel reactor is 9ml;
(2) Under the drive of the plunger pump of the power system, the raw material bromine is continuously introduced into the microchannel reactor at a flow rate of 0.5kg/min; Acetylene is continuously introduced into the microchannel reactor at a flow rate of 0.04kg/min through the gas mass flow controller; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor; The system pressure in the microchannel reactor is 0.1 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 2 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 98.5% and the yield is 98.3%.
Example 6:
A production process for preparing tetrabromoethane using a microchannel reactor:
(1) Micro-channel reactor: inner diameter of reaction channel is 1000um; The total volume of the reaction zone of the microchannel reactor is 45ml.
(2) Under the drive of the plunger pump of the power system, the raw material bromine is continuously introduced into the microchannel reactor at a flow rate of 0.8kg/min; Acetylene is continuously introduced into the microchannel reactor through the gas mass flow controller at a flow rate of 0.065kg/min; Before entering the microchannel reactor, acetylene and bromine flow through the valve group, which includes one-way valve, safety valve and switch.
(3) The incoming acetylene and bromine are fully mixed and reacted in the microchannel reactor, and the sunlight is increased. The sunlight is directly irradiated by a 40w fluorescent lamp at a close distance (about 20cm away from the microchannel reactor) (the higher the power of the fluorescent lamp, the more complete the tetrabromoethane reaction, the faster the color changes from light yellow to colorless, the better the effect); The system pressure in the microchannel reactor is 0.3 mpa; Control the temperature of reactants through the heat exchange system (the initial temperature is normal temperature, and maintain the reaction temperature ≤ 70 ℃); The residence time of the reactant in the microchannel reactor is 6 min.
(4) After the reaction process is completed, the product is collected through the gas-liquid separator. The content of tetrabromoethane is 99%, and the yield is 98.8%.
The production process of the invention can realize the safe reaction of bromine and acetylene, connect the control valve of raw acetylene and bromine with the computer software system, automatically feed after starting, effectively control the flow of bromine and acetylene to ensure the stability of the reaction between acetylene and bromine, and connect the heat exchange equipment instrument and the computer software in the microchannel reactor to effectively control the reaction temperature, reduce manual control, and realize automatic control, Improving production efficiency and yield can avoid the formation of explosive mixture of acetylene and air and improve the safety of reaction.