The application of 2,5-dimethoxytetrahydrofuran and the background and overview of the hydrolysis reaction cooling device
2,5-Dimethoxytetrahydrofuran is the raw material for the synthesis of tropinone. In the production process of tropinone, succinic acid obtained by hydrolysis of 2,5-dimethoxytetrahydrofuran is one of the raw materials for the synthesis of tropinone.
Application of 2,5-dimethoxytetrahydrofuran and hydrolysis reaction cooling device Hydrolysis reaction cooling device
The main equipment for the lithium tetrafluoroborate hydrolysis reaction of 2,5-dimethoxytetrahydrofuran is the reactor. It is known that the hydrolysis of 2,5-dimethoxytetrahydrofuran is an exothermic reaction. If the material is not cooled, The quality and yield of the product will be affected due to excessive temperature. Most of the existing reactors are cooled by passing ice salt water into a jacket set outside the reactor. However, the cooling effect of this reactor is average and cannot be used. Meet the temperature reduction requirements of the reaction system in the reactor.
CN201820570652.2 provides a cooling device during the hydrolysis reaction of 2,5-dimethoxytetrahydrofuran to achieve the purpose of rapidly cooling the materials in the reaction kettle. Figure 1 is a schematic diagram.
As shown in Figure 1, a cooling device during the hydrolysis reaction of 2,5-dimethoxytetrahydrofuran includes a reaction kettle 1, an interlayer 2 is provided outside the reaction kettle 1, and a cooling liquid inlet is provided on the upper part of the interlayer 2 , the lower part is provided with a coolant outlet, and the coolant is passed through the interlayer to cool down the reaction kettle 1. The upper part of the reactor 1 is equipped with a lid, and the lid is equipped with a feed port 3. The main reaction material 2,5-dimethoxytetrahydrofuran is passed into the kettle from the feed port 3, and the lower part of the reactor 1 is equipped with a discharge port. 4. The reaction kettle 1 is equipped with a stirring shaft 5 to ensure that the reaction materials are fully mixed; the 2,5-dimethoxytetrahydrofuran hydrolysis reaction is an exothermic reaction, and the cooling of the interlayer 2 alone cannot meet the requirements of the reaction system. temperature environment, so a coil 6 is installed inside the reaction kettle 1. The coil 6 is in a spiral shape. The spiral shape can effectively increase the contact area with the reaction liquid. The coolant inlet 61 of the coil 6 is located outside the upper part of the reactor 1, and the coolant outlet 62 is located outside the lower part of the reactor 1; the coolant inlet 61 is connected to the liquid storage tank 7 through a pipeline, and a pump 8 is provided on the pipeline; the coolant outlet 62 It is connected to the cooler 9 through a pipeline. The coolant takes away the heat of the reaction liquid in the kettle through the coil 6. The temperature of the coolant will rise, and the coolant flowing out from the coil outlet 62 needs to be cooled by the cooler 9. The cooler 9 is connected to the liquid storage tank 7 through a pipeline, transports the re-cooled coolant to the liquid storage tank 7, and pumps the coolant in the liquid storage tank 7 to the coil 6 inlet through the pump 8; the coolant inlet 61 A first valve 10 is provided between the coolant outlet 62 and the cooler 9 , and a second valve 11 is provided between the coolant outlet 62 and the cooler 9 . The valve can control the amount of coolant release according to actual reaction conditions.
In order to prevent the coil 6 from shaking during the cooling process, a fixed frame 12 is provided at the bottom of the reactor, and the coil 6 is fixed on the fixed frame to support the coil 6.
The kettle lid is provided with a temperature sensor 13 to facilitate real-time detection of the temperature inside the kettle to control the amount of coolant in and out.
The direction of the centerline of the coil 6 is consistent with the direction of the stirring shaft 5 to prevent the coil 6 from contacting the stirring shaft 5 during the stirring process.
The first valve 10 and the second valve 11 are solenoid valves, and the solenoid valves can control the amount of coolant more intelligently.
Coil 6 is a stainless steel coil, which has low cost and long service life.
The cooling liquid in the coil is ice salt water. Ice salt water has a better cooling effect than water and is also low in cost.
The working process of this utility model is: when starting the reaction, the reaction mixture is transported into the reaction kettle from the feed port on the kettle cover, and at the same time, ice brine is passed through the interlayer for interlayer cooling, and the pump pumps the liquid into the storage tank. The brine is pumped into the coil to cool the materials in the reaction kettle. The brine flowing out from the coil outlet is cooled twice by the cooler and then transported to the liquid storage tank through the pipeline, and the cycle continues; the temperature on the reaction kettle The sensor detects the reaction temperature in the kettle, based on which the solenoid valve can be used to control the delivery volume of the coolant.
Application of 2,5-dimethoxytetrahydrofuran and hydrolysis reaction cooling device
Application of 2,5-dimethoxytetrahydrofuran and application of hydrolysis reaction cooling device 1.
CN200810080248.8 reports an additive for improving the low-temperature startability of methanol diesel, consisting of 10 to 30 parts of ethyl acetate, 15 to 45 parts of dibutyl oxalate, 20 to 40 parts of diisoamyl oxalate, 0.3 to 5 10 parts of tertiary vinyl carbonate, 0.2~3 parts of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane, 7~20 parts of 2,5-dimethoxytetrahydrofuran, 2~ 15 parts of zirconium isooctanoate, 8~25 parts of 2-nitro-2-methylpropyl nitrate, 10~40 parts of 2-methoxyethyl nitrate, 15~30 parts of 3-tetrahydrofuran nitrate, 12~ 30 parts of methylbenzyl alcohol nitrate, 0.2~10 parts of 3-methyl-2-nitro-2-hexene, 0.2~10 parts of 3-ethyl-2-nitro-2-hexene, 0.1~10 parts It consists of 0 to 10 parts of barium nitrate, 0 to 10 parts of manganese dioxide, and 0 to 20 parts of potassium pentachloride. Mixing this additive into methanol diesel can improve the low-temperature startability of methanol diesel, make the combustion performance of methanol diesel better, and significantly improve exhaust emissions.
Application of 2,5-dimethoxytetrahydrofuran and application of hydrolysis reaction cooling device 2.
CN20181117 Trifluoromethoxypyridine 6.X discloses a two-dimensional polyphenylene ring bridgeThe preparation method of pyrrole relates to the field of two-dimensional carbon material preparation. The preparation method includes the following steps: first, add 2,5-dimethoxytetrahydrofuran, p-phenylenediamine and anhydrous copper chloride into a three-necked flask, Then add deionized water, drum N, and stir at constant temperature; then add ethyl acetate to the three-necked flask, filter, wash the filtrate with water, and rotary evaporate to obtain a solid crude product; use silica gel column chromatography to process the solid After the crude product, the benzene ring-bridged pyrrole monomer is obtained by rotary evaporation and vacuum drying. Finally, the benzene ring-bridged pyrrole monomer is oxidized and polymerized using acetone as the solvent and FeCl as the oxidizing agent to obtain a two-dimensional polyphenyl ring-bridged pyrrole; this method is gentle. Simple and low cost. The two-dimensional polyphenylene ring bridged pyrrole prepared by the invention has a nano-two-dimensional sheet structure, a nitrogen content of 6.5%, and has a specific capacity of up to 100F/g when used in supercapacitors.
References
[1] [China Utility Model] CN201820570652.2 A cooling device during the hydrolysis reaction of 2,5-dimethoxytetrahydrofuran
[2] [Chinese invention, Chinese invention authorization] CN200810080248.8 Additive for improving the low-temperature startability of methanol diesel oil
[3] [Chinese invention] CN201811176.X A two-dimensional polyphenyl ring bridged pyrrole and its preparation method
