Continuous tubular ozone oxidation reaction device suitable for gas-liquid mixing
Technical Field
The utility model belongs to the technical field of chemical reaction equipment, concretely relates to be applied to ozone oxidation serialization tubular reaction equipment in chemical industry, medicine field.
Background
Ozone oxidation is a clean oxidation technology, is a very important reaction in organic synthesis, has high yield and quick reaction, and has few side reactions. Because the ozone oxidation reaction is clean and efficient, the attention is paid more and more at present, most of the existing ozonization reaction still adopts the traditional stirring method, so that the high danger is caused, the temperature is difficult to control, the reaction is easy to explode, and meanwhile, the waste ozone is directly discharged into the air, so that the pollution is easy to cause. Tubular reaction continuous operation is adopted for ozone oxidation, the heat dissipation area is large, the temperature control is convenient, the safety and the efficiency are high, and meanwhile, residual ozone in reaction can be recycled.
The continuous tubular reactor is a new type of reactor, and compared with traditional stirring kettle, it has the following features that 1. the reactant molecules stay in the reactor for the same time, and the reactant concentration and chemical reaction speed at any point in the reactor do not change with time, but only with the length of the tube. 2. The tubular reactor has a large heat exchange surface per unit volume of the reactor, and is particularly suitable for reactions with large heat effect. 3. Its advantages are less back mixing of reactants in tubular reactor, high reaction speed and high flow speed, and high productivity. 4. The tubular reactor is suitable for large-scale and continuous chemical production. 5. Compared with a kettle reactor, the back mixing is small, and the flow pattern of the fluid in the pipe is close to the ideal inversion flow under the condition of low flow velocity. 6. The concentrations are not necessarily equal at all points in the tubular reactor, and the reaction rate varies depending on the spatial position. 7. Since the radial direction has a strictly uniform velocity profile, i.e. there is no concentration variation in the radial direction, the variation of the reaction rate with spatial position will be limited to the axial direction only. 8. The reaction results of the tubular reactor are uniquely determined by the chemical reaction kinetics. 9. The structure is simple and compact, the strength is high, the corrosion resistance is strong, the shock resistance is good, the service life is long, and the maintenance is convenient.
However, most of the existing tubular reactors are suitable for liquid-liquid reaction, including micro-channel technology generated by continuous process aiming at fine chemical production, which is emerging in recent years, and the gas-liquid mixing effect is poor. The utility model relates to a tubular reactor has the bubbling formula reaction characteristics concurrently, and it mixes to blow into gas from the below, adopts the screw stirring simultaneously, has overcome the not good problem of conventional tubular reactor gas-liquid mixture. Meanwhile, an anti-oxidation material is adopted, so that the corrosion of ozone to the reactor and the connecting pipe is avoided.
Disclosure of Invention
An object of the utility model is to provide an easy operation, safety ring protect, production efficiency is high, is applicable to the serialization tubular ozonation reaction unit of gas-liquid mixed situation to solve the problem that current equipment ozonization reaction gas-liquid mixes poorly, equipment is perishable, and the potential safety hazard is big.
The utility model relates to a continuation tubular ozone oxidation reaction unit, include: an ozone generator, a continuous tubular reactor with a propeller-driven agitator, a sample pump and a receiver; wherein, the left side of the tubular reactor is provided with a reaction liquid inlet, the lower part is provided with an ozone gas inlet, the right side is provided with a reaction liquid outlet, and the upper part is provided with a gas outlet; the sample injection pump is connected with a left inlet of the tubular reactor and is used for introducing reaction liquid; the ozone generator is connected with an inlet below the tubular reactor and is used for introducing ozone gas; the receiver is connected with a right outlet of the tubular reactor; the gas outlet above the tubular reactor is communicated with the inlet of the ozone generator, so that oxygen generated by the reaction and residual ozone are combined with an oxygen source, and the recycling is realized.
The utility model discloses in, each part material adopts one or more mixed materials such as hastelloy, stainless steel, tempered glass, nickel, chromium, carbon, silicon.
The utility model discloses in, the screw impels the agitator, and existing high-efficient gas-liquid mixture effect has serialization propulsive effect again.
In the utility model, the number of the tubular reactors can be 1, and a plurality of tubular reactors can be connected in series or in parallel.
The utility model discloses in, tubular reactor's internal diameter and length can be adjusted according to actual chemical reaction.
The utility model discloses in, the gas outlet department of tubular reactor top is provided with the check valve, connects ozone generator, recycles, not only practices thrift the cost but also protects the environment.
Compared with the prior art, the utility model mainly has the following characteristics:
1. the tubular reactor is adopted, so that the heat dissipation area is large, the tubular reactor is safer and controllable, and the industrial application of ozone oxidation is facilitated;
2. the tubular reactor is adopted, ozone is blown from the lower part and is mixed by a propeller, the ozone and reaction liquid are fully mixed by gas and liquid, the reaction efficiency is improved, the generation of byproducts is reduced, the ozone is fully utilized, and the cost is reduced;
3. the tubular reactor is adopted, and the residual ozone in the reaction is recycled through the one-way valve, so that the cost is reduced and the environment is protected;
4. and a continuous process is adopted, so that the energy consumption and the labor consumption of transfer during the operation of a conventional reaction kettle are avoided, the operation is simple and convenient, and the industrial mass production is facilitated.
Drawings
Fig. 1 is a structural diagram of the device of the present invention.
Reference numbers in the figures: 1 is an ozone generator, 2 is a tubular reactor, 3 is a sample injection pump, 4 is a receiver, 5 is a reaction liquid inlet, 6 is an ozone inlet, 7 is a reaction liquid outlet, 8 is a gas outlet, 9 is a one-way valve, and 10 is an oxygen inlet.
Detailed Description
The following embodiments better illustrate the present invention. However, the present invention is not limited to the following examples.
Example 1: as shown in figure 1, the utility model provides a serialization tubular reaction unit suitable for ozone oxidation reaction, including ozone generator 1, have screw propulsion stirring's tubular reactor 2, sampling pump 3 and receiver 4. The sampling pump 3 is connected with the left inlet 5 of the tubular reactor 2 and is filled with reaction liquid, the ozone generator 1 is connected with the lower inlet 6 of the tubular reactor 2 and is filled with ozone gas, the receiver 3 is connected with the right outlet 7 of the reaction, in addition, the gas outlet 8 above the reactor 2 is provided with a one-way valve 9 which can only be opened and closed and is communicated with the inlet of the ozone generator 1 and is combined with an oxygen source. The tubular reactor 2, the one-way valve 9, the propeller and the like are made of stainless steel-316 materials, and each connecting pipe is a butyl rubber pipe. The tubular reactor 2 has an internal diameter of 10cm and a length of 30cm, and the reaction time can be increased by connecting the reactors in series. The sample injection pump 3 and the ozone generator 1 are conventional sample injection pumps and ozone tube generators sold in the market.
Example 2: as shown in figure 1, the utility model provides a serialization tubular reaction unit suitable for ozone oxidation reaction, including ozone generator 1, have screw propulsion stirring's tubular reactor 2, sampling pump 3 and receiver 4. A sample pump 3 is connected with a left inlet 5 of a tubular reactor 2 and is filled with reaction liquid, an ozone generator 1 is connected with a lower inlet 6 of the tubular reactor 2 and is filled with ozone gas, a receiver 4 is connected with a right outlet 7 of the reactor, and a one-way valve 9 is arranged at a gas outlet 8 above the reactor 2 and is only not filled, communicated with an inlet of the ozone generator 1 and combined with oxygen. The tubular reactor, the one-way valve, the propeller and the like are made of Hastelloy materials, and all connecting pipes are in seamless connection by metal. The tubular reactor has an internal diameter of 5cm and a length of 20cm, and the reaction time can be increased by connecting the reactors in series. The sample injection pump 3 and the ozone generator 1 are conventional sample injection pumps and ozone tube generators sold in the market.
Example 3: as shown in figure 1, the utility model provides a serialization tubular reaction unit suitable for ozone oxidation reaction, including ozone generator 1, have screw propulsion stirring's tubular reactor 2, sampling pump 3 and receiver 4. The sampling pump 3 is connected with a left inlet 5 of the tubular reactor 2 and is filled with reaction liquid, the ozone generator 1 is connected with a lower inlet 6 of the tubular reactor 2 and is filled with ozone gas, the receiver 4 is connected with a right outlet 7 of the reactor 2, and in addition, a gas outlet above the reactor is a one-way valve and is only not filled, and is communicated with an inlet of the ozone generator and is combined with oxygen. The tubular reactor, the one-way valve, the propeller and the like are made of Mn/Si alloy materials, and the connecting pipes are linked by tetrafluoroethylene. The tubular reactor has an internal diameter of 2cm and a length of 15cm, and the reaction time can be increased by connecting the reactors in series. The sample injection pump 3 and the ozone generator 1 are conventional sample injection pumps and ozone tube generators sold in the market.
Performance evaluation: the performance tests of each example were performed using an anisic oil ozonation experiment comparing a conventional kettle reactor and a VMBHS0100 microreactor at the same temperature (room temperature) as shown in table 1 below.
TABLE 1
1. Compared with the conventional kettle type reactor, the utility model has the advantages that the ozone flux can be reacted only by 2mL, the ozone utilization rate is greatly improved compared with the traditional kettle type reactor, the yield is obviously higher than that of the kettle type reactor, and byproducts are reduced;
2. compared with a VMBHS0100 micro-reactor, the reaction time of the utility model is greatly shortened because the gas-liquid mixing effect is greatly improved compared with the traditional micro-reactor, and meanwhile, the yield is almost consistent;
3. the utility model discloses possess and improve reaction efficiency, reduce the production of accessory substance, make full use of ozone, reduce cost, serialization technology more is applicable to the characteristics of industrialization.