Reaction device for preparing ester base oil in laboratory
By designing an apparatus for esterification reactions and using gas supply and extraction devices to control reaction conditions, the problem of low reaction rates in esterification apparatus under heating, pressurization, or vacuum conditions was solved, thereby improving product conversion rate and apparatus efficiency.
Patent Information
- Application Number
- CN202520094448.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-15
- Publication Date
- 2026-02-24
- Estimated Expiration
- 2035-01-15
AI Technical Summary
In existing technologies, esterification reaction devices cannot simultaneously perform heating and pressurization or heating and vacuum tests, resulting in low reaction rates and low product conversion rates. Furthermore, traditional dehydrating agents are ineffective, increasing material and post-processing costs.
Design a reaction device that produces nitrogen gas through a gas supply device and sends it into the reaction device, combines it with a gas extraction device to rapidly evaporate moisture, controls the heating and cooling rates, and achieves pressurization or depressurization to improve the gas stripping rate and product conversion rate.
It achieves accurate temperature control of the reaction, improves gas stripping rate and product conversion rate, is easy to use, and reduces material consumption and post-processing costs.
Smart Images
Figure CN223931388U_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the technical field of preparing ester base oils, and in particular to a reaction apparatus for the laboratory preparation of ester base oils. Background Technology
[0002] To improve the reaction rate and conversion rate of the target product in esterification, chemical industrial production has adopted methods such as increasing the concentration of reactants and adding a small amount of dehydrating agent to increase the reaction rate and esterification rate. However, increasing the concentration of reactants increases losses and has low efficiency. Common dehydrating agents are not very effective and increase material and post-processing costs, making it impossible to achieve greater efficiency and higher degree of dehydration. In addition, many reaction devices cannot simultaneously perform heating and pressurization or heating and vacuum tests.
[0003] The device in this case can be tested under pressure or vacuum. It can be pressurized and stripped of moisture by introducing dry inert gas, or dehydrated by vacuum suction and decompression, so that the water generated in the reaction can be removed in a timely and rapid manner. Utility Model Content
[0004] To solve the above-mentioned technical problems, this utility model provides a reaction apparatus for the laboratory preparation of ester base oils. The apparatus generates nitrogen gas through a gas supply device and feeds it into a reaction device, which provides reaction space for the materials and maintains temperature and stirring. A vacuum device rapidly evaporates the water produced during the reaction. By simultaneously controlling the heating and cooling rates, the reaction temperature is accurately controlled. The apparatus can be pressurized or depressurized, has a high gas stripping rate, a high product conversion rate, and is easy to use.
[0005] This invention relates to a reaction apparatus for the laboratory preparation of ester base oils; it includes a gas supply device, a reaction device, and a gas extraction device. The reaction device is connected to the gas supply device, and the gas extraction device is connected to the reaction device. Nitrogen gas is produced by the gas supply device and sent into the reaction device. The reaction device provides reaction space for the materials and maintains the temperature and stirring. The gas extraction device rapidly evaporates the water produced in the reaction. By simultaneously controlling the heating and cooling rates, the reaction temperature is accurately controlled. The reaction can be pressurized or depressurized, with a high gas stripping rate, high product conversion rate, and convenient use.
[0006] Preferably, the gas supply device includes an air compressor, a first transparent gas delivery pipe, a nitrogen generator, a liquid level display window, a pressure gauge, a flow rate display, a control switch, a gas distributor, and a second transparent gas delivery pipe. The input end of the nitrogen generator is connected to the air compressor via the first transparent gas delivery pipe. A gas distributor is installed on the output end of the nitrogen generator, and the output end of the gas distributor is connected to the second transparent gas delivery pipe. The nitrogen generator is equipped with a liquid level display window, a pressure gauge, a flow rate display, and a control switch. Outside air is supplied to the nitrogen generator by the air compressor, and nitrogen is produced by the nitrogen generator. The gas distributor ensures that the gas output from the nitrogen generator is evenly distributed. The uniform diffusion of gas into the reaction system helps to promptly remove dissolved oxygen and water vapor generated during the stripping reaction. A liquid level display window allows operators to easily monitor the liquid level, a pressure gauge allows them to monitor the internal gas pressure, a flow meter allows them to monitor the real-time flow, and a control switch allows them to easily control the equipment. The gas supply device delivers dry nitrogen into the reaction apparatus, improving the gas stripping rate and product conversion rate. Replacing traditional nitrogen cylinders with a nitrogen generator provides a continuous supply of dry nitrogen. The equipment is small, lightweight, has a long operating cycle, and is stable and reliable, enhancing its practicality.
[0007] Preferably, the reaction apparatus includes a three-necked round-bottom flask, a digital display thermostatic magnetic stirrer, a heating mantle, a spherical condenser, a first thermometer, a distillation head, and a second thermometer. The heating mantle is mounted on the upper surface of the digital display thermostatic magnetic stirrer, and a groove is provided on the heating mantle. The three-necked round-bottom flask is placed in the groove on the heating mantle. The lower part of the spherical condenser is connected to the upper middle opening of the three-necked round-bottom flask. The output end of the second transparent gas delivery tube communicates with the interior of the three-necked round-bottom flask through one side opening. The first thermometer consists of three... Another port on the three-necked round-bottom flask is inserted into the three-necked round-bottom flask. The upper part of the spherical condenser is connected to the distillation head, and a second thermometer is inserted into the top port of the distillation head. A polytetrafluoroethylene stopcock valve is installed on the distillation head. The material in the three-necked round-bottom flask is stirred and assisted in heating by a digital display constant temperature magnetic stirrer. The steam generated by heating is condensed once by the spherical condenser. The liquid temperature in the three-necked round-bottom flask is monitored by the first thermometer, and the steam temperature is monitored by the second thermometer.
[0008] Preferably, the extraction device includes a straight condenser, a bulltail-shaped vacuum receiving tube, a collection bottle, a transparent silicone tube, and a vacuum pump. The straight condenser is connected to the side port of the distillation head, the bulltail-shaped vacuum receiving tube is connected to the output end of the straight condenser, the collection bottle is connected to the lower port of the bulltail-shaped vacuum receiving tube, and the transparent silicone tube is connected to the side port of the bulltail-shaped vacuum receiving tube. The transparent silicone tube is connected to the vacuum pump. The reaction gas is extracted by the vacuum pump in conjunction with the transparent silicone tube. The cooling reflux rate of carboxylic acid vapor by the spherical condenser can be controlled by adjusting the temperature and flow rate of the heat transfer oil, and the condensation rate of water vapor by the straight condenser can be controlled by adjusting the temperature and flow rate of the cooling water, thus improving the practicality of the equipment.
[0009] Preferably, the glass instrument connections are lubricated and sealed with high-vacuum silicone grease. By using high-vacuum silicone grease to lubricate and seal the glass instrument connections, the airtightness of the reaction equipment is increased, the pollution of the operating environment caused by the leakage of reaction gases during the reaction process is reduced, and the practicality of the device is improved.
[0010] Preferably, the device also includes a connection between the middle neck of the three-necked round-bottom flask and the lower end of the spherical condenser tube. The neck of the three-necked round-bottom flask is clamped with a flask clamp, and the spherical condenser tube and the straight condenser tube are fixed at a position slightly below the middle with a condenser tube clamp. The flask clamp and the condenser tube clamp fix the glass components of the equipment, preventing them from loosening and falling off due to vibration of the equipment itself during the reaction process, thereby improving the stability and practicality of the device.
[0011] Preferably, the vacuum pump is also equipped with a valve and a shock-resistant vacuum pressure gauge; the valve on the vacuum pump allows the operator to quickly control the working status of the vacuum pump and control the pumping rate, while the shock-resistant vacuum pressure gauge allows the operator to observe the negative pressure inside the equipment, so as to control the reaction rate and improve the practicality of the device.
[0012] Compared with the prior art, the advantages of this utility model are as follows: nitrogen gas is produced by the gas supply device and sent into the reaction device; the reaction device provides reaction space for the materials and maintains the temperature and stirring; the water generated by the reaction is quickly evaporated by the gas extraction device; the reaction temperature is accurately controlled by simultaneously controlling the heating rate and cooling rate; the reaction can be pressurized or depressurized; the gas stripping rate is high; the product conversion rate is high; and it is easy to use. Attached Figure Description
[0013] Figure 1 This is a schematic diagram of the structure of this utility model;
[0014] Figure 2 This is an isometric structural diagram of the nitrogen generator of this utility model;
[0015] The attached diagram is labeled as follows: 1. Air compressor; 2. First transparent gas delivery pipe; 3. Nitrogen generator; 4. Liquid level display window; 5. Pressure gauge; 6. Flow rate display; 7. Control switch; 8. Gas distributor; 9. Second transparent gas delivery pipe; 10. Three-necked round-bottom flask; 11. Digital display constant temperature magnetic stirrer; 12. Heating mantle; 13. Spherical condenser; 14. First thermometer; 15. Distillation head; 16. Second thermometer; 17. Straight condenser; 18. Bull's tail vacuum receiving tube; 19. Collection bottle; 20. Transparent silicone tube; 21. Vacuum pump. Detailed Implementation
[0016] To facilitate understanding of this utility model, a more complete description will be given below with reference to the accompanying drawings. This utility model can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to make the disclosure of this utility model more thorough and complete.
[0017] Example 1
[0018] Figure 1 , Figure 2 As shown, the reaction device is connected to the gas supply device, and the gas extraction device is connected to the reaction device.
[0019] First, the air compressor 1 is turned on to send outside gas into the nitrogen generator 3 through the first transparent gas delivery pipe 2. Then, the nitrogen generator 3 is turned on to produce dry nitrogen gas, which is delivered to the three-necked round-bottom flask 10 through the second transparent gas delivery pipe 9. Then, the digital display constant temperature magnetic stirrer 11 is turned on to drive the magnetic block inside the three-necked round-bottom flask 10 to rotate, thereby stirring the material inside the three-necked round-bottom flask 10 and heating the three-necked round-bottom flask 10 to increase the reaction temperature. Then, the gas produced enters the straight condenser 17 through the spherical condenser 13. Then, the vacuum pump 21 is turned on to extract the gas in the equipment to maintain the required negative pressure state.
[0020] The gas delivery device includes an air compressor 1, a first transparent gas delivery pipe 2, a nitrogen generator 3, a liquid level display window 4, a pressure indicator 5, a flow rate display 6, a control switch 7, a gas distributor 8, and a second transparent gas delivery pipe 9. The input end of the nitrogen generator 3 is connected to the air compressor 1 through the first transparent gas delivery pipe 2. The output end of the nitrogen generator 3 is equipped with a gas distributor 8, and the output end of the gas distributor 8 is connected to the second transparent gas delivery pipe 9. The nitrogen generator 3 is equipped with a liquid level display window 4, a pressure indicator 5, a flow rate display 6, and a control switch 7.
[0021] The reaction apparatus includes a three-necked round-bottom flask 10, a digital display constant-temperature magnetic stirrer 11, a heating mantle 12, a spherical condenser 13, a first thermometer 14, a distillation head 15, and a second thermometer 16. The heating mantle 12 is mounted on the upper surface of the digital display constant-temperature magnetic stirrer 11. The heating mantle 12 has a groove. The three-necked round-bottom flask 10 is placed in the groove on the heating mantle 12. The lower part of the spherical condenser 13 is connected to the upper middle opening of the three-necked round-bottom flask 10. The output end of the second transparent gas delivery tube 9 is connected to the inside of the three-necked round-bottom flask 10 through one side opening. The first thermometer 14 is inserted into the inside of the three-necked round-bottom flask 10 from the other port. The upper part of the spherical condenser 13 is connected to the distillation head 15. The second thermometer 16 is inserted into the top port of the distillation head 15. A polytetrafluoroethylene stopcock valve is provided on the distillation head 15.
[0022] The vacuum pumping device includes a straight condenser tube 17, a cowtail-shaped vacuum receiving tube 18, a collection bottle 19, a transparent silicone tube 20, and a vacuum pump 21. The straight condenser tube 17 is connected to the side port of the distillation head 15. The cowtail-shaped vacuum receiving tube 18 is connected to the output end of the straight condenser tube 17. The collection bottle 19 is connected to the lower port of the cowtail-shaped vacuum receiving tube 18. The transparent silicone tube 20 is connected to the side port of the cowtail-shaped vacuum receiving tube 18. The transparent silicone tube 20 is connected to the vacuum pump 21.
[0023] This also includes the use of high-vacuum silicone grease for lubrication and sealing of ground joints at glass instrument connections;
[0024] It also includes the connection between the middle mouth of the three-necked round-bottom flask 10 and the lower end of the spherical condenser tube 13, the neck of the three-necked round-bottom flask 10 is clamped with flask clamps, and the spherical condenser tube 13 and the straight condenser tube 17 are fixed at the lower middle position with condenser tube clamps.
[0025] It also includes a valve and a shock-resistant vacuum pressure gauge installed on the vacuum pump 21;
[0026] Nitrogen gas is produced by a gas supply device and fed into the reaction device. The reaction device provides reaction space for the materials and maintains the temperature and stirring. The water produced in the reaction is quickly evaporated by a gas extraction device. By controlling the heating rate and cooling rate simultaneously, the reaction temperature is accurately controlled. The reaction can be pressurized or depressurized. The gas stripping rate is high, the product conversion rate is high, and it is easy to use.
[0027] like Figures 1 to 2As shown, this utility model discloses a reaction apparatus for the laboratory preparation of ester base oils. During operation, the air compressor 1 is first turned on to send external gas into the nitrogen generator 3 through the first transparent gas delivery pipe 2. Then, the nitrogen generator 3 is turned on to produce dry nitrogen gas, which is delivered to the three-necked round-bottom flask 10 through the second transparent gas delivery pipe 9. Next, the digital display constant-temperature magnetic stirrer 11 is turned on to rotate the magnetic block inside the three-necked round-bottom flask 10, thereby stirring the material inside the flask and simultaneously heating the flask 10 to increase the reaction temperature. The produced gas then enters the straight condenser 17 through the spherical condenser 13. Finally, the vacuum pump 21 is turned on to extract the gas from the equipment to maintain the required negative pressure.
[0028] The air compressor 1, nitrogen generator 3, digital display constant temperature magnetic stirrer 11, and vacuum pump 21 of the reaction apparatus for preparing ester base oils in the laboratory of this utility model are commercially available. Technical personnel in this industry only need to install and operate them according to the accompanying instruction manual, without requiring any creative work from those skilled in the art.
[0029] The above description is only a preferred embodiment of the present utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present utility model, and these improvements and modifications should also be considered within the protection scope of the present utility model.
Claims
1. A reaction apparatus for the laboratory preparation of ester base oils; characterized in that, It includes a gas supply device, a reaction device, and a gas extraction device. The reaction device is connected to the gas supply device, and the gas extraction device is connected to the reaction device. The gas supply device includes an air compressor (1), a first transparent gas supply pipe (2), a nitrogen generator (3), a liquid level display window (4), a pressure indicator (5), a flow rate display (6), a control switch (7), a gas distributor (8), and a second transparent gas supply pipe (9). The input end of the nitrogen generator (3) is connected to the air compressor (1) through the first transparent gas supply pipe (2). The output end of the nitrogen generator (3) is equipped with a gas distributor (8). The output end of the gas distributor (8) is connected to the second transparent gas supply pipe (9). The nitrogen generator (3) is equipped with a liquid level display window (4), a pressure indicator (5), a flow rate display (6), and a control switch (7).
2. The reaction apparatus for the laboratory preparation of ester base oils as described in claim 1, characterized in that, The reaction apparatus includes a three-necked round-bottom flask (10), a digital display constant-temperature magnetic stirrer (11), a heating mantle (12), a spherical condenser (13), a first thermometer (14), a distillation head (15), and a second thermometer (16). A heating mantle (12) is mounted on the upper surface of the digital display constant-temperature magnetic stirrer (11). A groove is provided on the heating mantle (12), and the three-necked round-bottom flask (10) is placed in the groove on the heating mantle (12). The lower part of the spherical condenser (13) is connected to the three-necked round-bottom flask (10). 0) The upper middle part is connected, and the output end of the second transparent gas supply tube (9) is connected to the inside of the three-necked round bottom flask (10) through one side port. The first thermometer (14) is inserted into the inside of the three-necked round bottom flask (10) through the other port. The upper part of the spherical condenser tube (13) is connected to the distillation head (15). The second thermometer (16) is inserted into the top port of the distillation head (15). A polytetrafluoroethylene stopcock valve is provided on the distillation head (15).
3. The reaction apparatus for laboratory preparation of ester base oils as described in claim 2, characterized in that, The vacuum pump includes a straight condenser (17), a cowtail-shaped vacuum receiving tube (18), a collection bottle (19), a transparent silicone tube (20), and a vacuum pump (21). The straight condenser (17) is connected to the side port of the distillation head (15). The cowtail-shaped vacuum receiving tube (18) is connected to the output end of the straight condenser (17). The collection bottle (19) is connected to the lower port of the cowtail-shaped vacuum receiving tube (18). The transparent silicone tube (20) is connected to the side port of the cowtail-shaped vacuum receiving tube (18). The transparent silicone tube (20) is connected to the vacuum pump (21).
4. The reaction apparatus for laboratory preparation of ester base oils as described in claim 3, characterized in that, This also includes the use of high-vacuum silicone grease for lubrication and sealing of ground joints at glass instrument connections.
5. The reaction apparatus for laboratory preparation of ester base oils as described in claim 4, characterized in that, It also includes the connection between the middle mouth of the three-necked round-bottom flask (10) and the lower end of the spherical condenser (13), the neck of the three-necked round-bottom flask (10) is clamped with flask clamps, and the lower part of the middle of the spherical condenser (13) and the straight condenser (17) is fixed with condenser clamps.
6. The reaction apparatus for laboratory preparation of ester base oils as described in claim 5, characterized in that, It also includes a vacuum pump (21) equipped with a valve and a shock-resistant vacuum pressure gauge.