A continuous production device and method for synthesizing borneol from camphor
By using continuous production equipment and high-strength granular nickel catalysts, the problems of low yield, low selectivity and environmental pollution in the synthetic borneol process were solved, and efficient and safe borneol production was achieved.
Patent Information
- Application Number
- CN202310828206.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-07
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2043-07-07
AI Technical Summary
The existing borneol synthesis process has low yield and selectivity of the esterification reaction, the catalyst cannot be reused, post-processing is difficult, wastewater treatment is complicated, there is a risk of fire and explosion, pollution is serious, and the production cycle is long.
A continuous production device is used, including camphor storage tanks, hydrogen storage tanks, fixed-bed reactors, gas-liquid separators and distillation towers. Through liquid and gas phase circulation conveying components, condensers and transfer pumps, high-strength granular nickel catalysts and automated control are used to achieve continuous hydrogenation, concentration, crystallization and centrifugation of camphor.
The yield and quality of borneol are improved, the production cycle and risk are shortened, environmental pollution is reduced, the operation process is simplified, and the stability and safety of the product are achieved.
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Figure CN116850901B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of organic synthesis, and particularly relates to a continuous production device and method for synthesizing borneol from camphor. BACKGROUND
[0002] Borneol is colorless transparent or white translucent flaky crisp crystal, has volatility, gas is fragrant, tastes bitter, cool; and is dissolved in most organic solvents, such as ethanol, chloroform, gasoline or diethyl ether, etc., is almost insoluble in water, synthetic borneol mainly contains borneol 59.78%~58.93%, isoborneol 38.98%~37.52%, camphor 2.70%~2.09%. Synthetic borneol has special smell similar to camphor and mint, and is also an important chemical raw material, and is widely used in spices, traditional Chinese medicine, food, high-grade perfume, insect repellent and various fields. Compared with natural borneol, synthetic borneol often contains n-borneol and isoborneol, and the higher the content of n-borneol is, the better the medicinal value is.
[0003] Industrial production of synthetic borneol mainly uses pine oil containing pinene as raw material, and esterification reaction is carried out under different types of catalyst systems with anhydrous oxalic acid, chloroacetic acid and the like, and then borneol acetate is converted, and then saponification hydrolysis is carried out to obtain high value borneol. However, in the traditional method, the esterification reaction has low yield and low selectivity, which leads to low borneol content in the saponification product, and seriously affects the quality of synthetic borneol; the esterification catalyst cannot be reused, and the post-treatment is difficult, and the solid waste generated cannot be recycled, which pollutes the environment. The existing esterification reaction generally uses boric anhydride as a catalyst, and esterification reaction is carried out with a-pinene and oxalic acid, the esterification time is long, the production cycle is long, the temperature control requirement is extremely strict, and once out of control, improper handling is easy to cause fire and explosion.
[0004] In addition, another deficiency of the existing process is that the wastewater after esterification reaction is difficult to treat: the water phase containing organic and inorganic acids such as oxalic acid and boric acid cannot be directly discharged, the treatment process is complicated, and the cost of wastewater treatment offsets most of the product profit; in addition, 120# gasoline is used as a solvent in the crude crystallization, and because a large amount of high-grade gasoline is used for a long time, there is high pollution and high risk of causing fire and explosion, and the gasoline vapor seriously pollutes the environment and harms the health of workers. SUMMARY
[0005] The present application aims to provide a continuous production device and method for synthesizing borneol from camphor to solve the problems in the background art.
[0006] To achieve the above-mentioned purpose, the present application provides the following technical scheme: a continuous production device for synthesizing borneol from camphor, comprising a camphor storage tank, a hydrogen storage tank, a fixed bed reactor, a gas-liquid separator and a rectifying column, further comprising:
[0007] a gas-liquid mixer, wherein the output end of the gas-liquid mixer is connected to the input end of the fixed bed reactor, the liquid phase input end of the gas-liquid mixer is connected to a liquid phase preheater, a liquid phase circulation and delivery component is provided between the camphor storage tank, the liquid phase preheater, and the distillation tower, the gas phase input end of the gas-liquid mixer is connected to the gas phase preheater, and a gas phase circulation and delivery component is provided between the hydrogen storage tank, the gas phase preheater, and the gas-liquid separator;
[0008] a condenser, the condenser being disposed between the fixed bed reactor and the gas-liquid separator, the input end of the condenser being connected to the output end of the fixed bed reactor, and the output end of the condenser being connected to the input end of the gas-liquid separator;
[0009] an intermediate storage tank, which is disposed between the gas-liquid separator and the distillation tower, wherein the input end of the intermediate storage tank is connected to the output end of the gas-liquid separator, and the output end of the intermediate storage tank is connected to the input end of the distillation tower;
[0010] A material transfer pump is connected to the output end of the tower kettle of the distillation tower.
[0011] It should be noted that the liquid phase circulation and delivery component includes:
[0012] a solvent storage tank, wherein the input end of the solvent storage tank is connected to the liquid phase output end of the distillation tower, the output end of the solvent storage tank is connected to a solvent delivery pump, the output end of the solvent delivery pump and the output end of the camphor storage tank are commonly connected to a heating ingredient kettle, and the output end of the heating ingredient kettle is connected to a liquid phase delivery pump;
[0013] A liquid flow meter, wherein the input end of the liquid flow meter is connected to the output end of the liquid phase delivery pump, and the output end of the liquid flow meter is connected to the input end of the liquid phase preheater.
[0014] It is further worth noting that the gas phase circulation conveying component includes:
[0015] a hydrogen compressor, wherein the input end of the hydrogen compressor is connected to the output end of the hydrogen storage tank;
[0016] A circulating gas compressor, the input end of the circulating gas compressor is connected to the gas phase output end of the gas-liquid separator, the output end of the circulating gas compressor and the output end of the hydrogen compressor are commonly connected to a gas flow meter, and the output end of the gas flow meter is connected to the input end of the gas phase preheater.
[0017] A continuous production method for synthesizing borneol from camphor, based on a continuous production device, comprises the following steps:
[0018] S1, camphor hydrogenation reaction: first catalyst is loaded into the pressure-resistant fixed-bed reactor with heating, and use nitrogen replacement, ensure that the device is absolutely oxygen-free, then open the fixed-bed reactor heating unit, the fixed-bed reactor temperature is maintained under reaction conditions, camphor solution enters from camphor storage tank into the liquid phase circulation conveying assembly and carries out batching and dissolving and is delivered to liquid phase preheater for preheating treatment, simultaneously hydrogen enters from hydrogen storage tank in the gas phase circulation conveying assembly and is compressed and is delivered to gas phase preheater for preheating treatment, together send into gas-liquid mixer and mix uniformly, finally from fixed-bed reactor top, send into fixed-bed reactor, carry out hydrogenation reaction;
[0019] S2, gas-liquid separation: after the material coming out of the end of the fixed-bed reactor in step S1 enters the condenser, it enters the gas-liquid separator for gas-liquid separation, the separated hydrogen is transported by the gas phase compressor and merged with the new hydrogen sent by the hydrogen compressor, and then preheated in the gas phase preheater, enters the gas-liquid mixer and is mixed with the ethanol camphor solution from the liquid phase preheater, and then returns to the fixed-bed reactor for cyclic hydrogenation reaction;
[0020] S3, distillation separation: the material after gas-liquid separation in the gas-liquid separator in step S2 reaches the intermediate storage tank and then enters the continuous distillation tower for separation. Most of the reaction solvent at the top of the distillation tower is recovered and circulated into the solvent storage tank. The crude borneol in the bottom of the tower is transported to the freezing crystallization device through a transfer pump, and the crude borneol is obtained through freezing, crystallization and centrifugation.
[0021] It should be noted in the scheme that the concentration of the liquid solution in the heating batching kettle is 10%-80%, and the preheating temperature of the liquid preheater is 60°C-180°C.
[0022] It is further worth mentioning that the preheating temperature in the gas phase preheater is 100°C-200°C.
[0023] It should be further noted that the gas phase flow rate of the fixed bed reactor is 800m 3 / h-1000m 3 / h, liquid phase flow rate is 0.1m 3 / h-0.5m 3 / h, gas-liquid ratio is 1600-10000.
[0024] As a preferred embodiment, the reaction temperature in the fixed bed reactor is 120°C
[0025] -200℃, reaction pressure is 1MPa-5MPa.
[0026] Compared with the prior art, the present invention provides a continuous production device and method for synthesizing borneol from camphor, which has at least the following beneficial effects:
[0027] (1) Camphor is directly used as raw material, and high-quality crude borneol can be obtained through continuous hydrogenation, concentration, crystallization, and centrifugation. This process has a short production cycle, low risk factor, and no harm to the environment. In addition, the process is simple to operate and has few reaction steps.
[0028] (2) The fixed-bed reactor continuous hydrogenation production device and method improves the unstable state in hydrogenation production and effectively improves production efficiency. It is convenient to use an automatic control system in the production process, greatly reducing the product process instability caused by human operation deviations, so that the hydrogenation production process can meet the requirements of stable product quality, safety, high efficiency and low consumption. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 Schematic diagram of the device structure of the present invention.
[0030] In the figure: 1. Camphor storage tank; 2. Hydrogen storage tank; 3. Fixed bed reactor; 4. Gas-liquid separator; 5. Distillation tower; 6. Gas-liquid mixer; 7. Liquid preheater; 8. Liquid circulation and conveying assembly; 81. Solvent storage tank; 82. Solvent delivery pump; 83. Heating and batching kettle; 84. Liquid delivery pump; 85. Liquid flow meter; 9. Gas preheater; 10. Gas circulation and conveying assembly; 101. Hydrogen compressor; 102. Circulating gas compressor; 103. Gas flow meter; 11. Condenser; 12. Intermediate storage tank; 13. Transfer pump. DETAILED DESCRIPTION
[0031] The present invention will be further described below with reference to the embodiments.
[0032] See also Figure 1 The present invention provides a continuous production device for synthesizing borneol from camphor, comprising a camphor storage tank 1, a hydrogen storage tank 2, a fixed bed reactor 3, a gas-liquid separator 4 and a distillation tower 5, and further comprising a gas-liquid mixer 6, wherein the output end of the gas-liquid mixer 6 is connected to the input end of the fixed bed reactor 3, the liquid phase input end of the gas-liquid mixer 6 is connected to a liquid phase preheater 7, a liquid phase circulation conveying component 8 is provided between the camphor storage tank 1, the liquid phase preheater 7 and the distillation tower 5, the gas phase input end of the gas-liquid mixer 6 is connected to a gas phase preheater 9, and a gas phase circulation conveying component 10 is provided between the hydrogen storage tank 2, the gas phase preheater 9 and the gas-liquid separator 4;
[0033] The condenser 11 is arranged between the fixed bed reactor 3 and the gas-liquid separator 4. The input end of the condenser 11 is connected to the output end of the fixed bed reactor 3, and the output end of the condenser 11 is connected to the input end of the gas-liquid separator 4.
[0034] The intermediate storage tank 12 is provided between the gas-liquid separator 4 and the distillation tower 5, the input end of the intermediate storage tank 12 is connected to the output end of the gas-liquid separator 4, and the output end of the intermediate storage tank 12 is connected to the input end of the distillation tower 5;
[0035] The material transfer pump 13 is connected to the output end of the tower bottom of the distillation tower 5.
[0036] It is worth noting that the fixed bed reactor 3 is preferably cylindrical, with a screen inside for fixing the catalyst. The catalyst is added to the fixed bed reactor 3 at one time, and its service life is about 6-12 months. The catalyst filling mass is 200kg-1000kg. A temperature sensor and a pressure sensor are provided in the fixed bed reactor 3; a heating and cooling jacket is provided on the outer periphery of the fixed bed reactor 3, and the inlet of the heating and cooling jacket is connected to the heating medium pipe and the cooling medium pipe through a branch pipe equipped with a valve. The heating heat source can be electricity, superheated water steam or thermal oil.
[0037] By selecting high-strength granular nickel as the reaction catalyst, the catalytic activity for camphor hydrogenation is high, and it is inexpensive, stable, and has good regeneration performance. Its service life is as long as 6-12 months, which solves the problems of short catalyst life, increased costs caused by repeated catalyst replacement during production, and low equipment utilization. In addition, the use of automated control of the hydrogenation production process makes the catalytic reaction highly selective, and camphor can be effectively converted into borneol and isoborneol.
[0038] The gas-liquid mixer 6 can be a spray type, a pipeline type gas-liquid mixer 6, etc. Its main purpose is to mix the hydrogen and the materials evenly so that the materials are fully contacted during the reaction process.
[0039] The liquid phase preheater 7 can be a shell-and-tube heat exchanger, a shell-and-tube heat exchanger or a plate heat exchanger, and its heat exchange area is determined by heat balance according to the production capacity.
[0040] The gas phase preheater 9 can be a shell-and-tube heat exchanger, a shell-and-tube heat exchanger, a plate heat exchanger or a plate-fin heat exchanger, and its heat exchange area is determined by heat balance according to the production capacity.
[0041] The condenser 11 may be a tubular heat exchanger or a plate heat exchanger, and its heat exchange area is determined by heat balance according to the production capacity.
[0042] It is worth noting that the solvent storage tank 81 preferably contains an ethanol solvent, which may be an alcohol solvent such as methanol or isopropanol, or a saturated alkane or cycloalkane such as heptane, cyclohexane, or p-menane, or a saturated heterocyclic compound such as tetrahydrofuran or dioxane, or a mixture thereof;
[0043] It is worth noting that the liquid phase circulation conveying component 8 includes a solvent storage tank 81, the input end of the solvent storage tank 81 is connected to the liquid phase output end of the distillation tower 5, the output end of the solvent storage tank 81 is connected to a solvent delivery pump 82, the output end of the solvent delivery pump 82 and the output end of the camphor storage tank 1 are commonly connected to a heating ingredient kettle 83, and the output end of the heating ingredient kettle 83 is connected to a liquid phase delivery pump 84;
[0044] The liquid flow meter 85 has an input end connected to the output end of the liquid phase delivery pump 84 , and an output end of the liquid flow meter 85 is connected to the input end of the liquid phase preheater 7 .
[0045] It is worth noting that the gas phase circulation transport component 10 includes a hydrogen compressor 101, and the input end of the hydrogen compressor 101 is connected to the output end of the hydrogen storage tank 2;
[0046] The circulating gas compressor 102 has an input end connected to the gas phase output end of the gas-liquid separator 4, and the output end of the circulating gas compressor 102 and the output end of the hydrogen compressor 101 are commonly connected to a gas flow meter 103, and the output end of the gas flow meter 103 is connected to the input end of the gas phase preheater 9.
[0047] It is worth noting that the liquid phase preheater 7, hydrogen storage tank 2, hydrogen compressor 101, circulating gas compressor 102, gas phase preheater 9, gas-liquid mixer 6, fixed bed reactor 3 and distillation tower 5 are respectively provided with temperature sensors or pressure sensors or flow sensors. The temperature sensors, pressure sensors and flow sensors are all connected to the computer center. The process parameter information of all production processes is transmitted to the computer center through the pressure, temperature or flow sensors of each control point to implement continuous production and fully automatic control.
[0048] A continuous production method for synthesizing borneol from camphor is based on a continuous production device and comprises the following steps:
[0049] S1, camphor hydrogenation reaction: first catalyst is packed into the pressure-resistant fixed-bed reactor 3 with heating, and use nitrogen replacement, ensure that device is absolutely anaerobic, then open fixed-bed reactor 3 heating units, fixed-bed reactor 3 temperature is maintained at reaction conditions, camphor solution enters into liquid-phase circulation conveying assembly 8 from camphor storage tank 1 and carries out batching and dissolving and is delivered to liquid-phase preheater 7 for preheating treatment, simultaneously hydrogen enters gas-phase circulation conveying assembly 10 from hydrogen storage tank 2 and is compressed and is sent into gas-phase preheater 9 for preheating treatment, send into together in gas-liquid mixer 6 and mix, finally from fixed-bed reactor 3 top, send into fixed-bed reactor 3, carry out hydrogenation;
[0050] S2, gas-liquid separation: after the material coming out of the end of step S1 fixed-bed reactor 3 enters condenser 11, enters gas-liquid separator 4 for gas-liquid separation, the separated hydrogen is transported by gas phase compressor and merged with the new hydrogen sent by hydrogen compressor 101, and then preheated by gas phase preheater 9, enters gas-liquid mixer 6 and mixes with the ethanol camphor solution from liquid phase preheater 7, and then returns to fixed-bed reactor 3 for cyclic hydrogenation reaction;
[0051] S3, distillation separation: The material after gas-liquid separation in the gas-liquid separator 4 in step S2 reaches the intermediate storage tank 12 and then enters the continuous distillation tower 5 for separation. Most of the reaction solvent at the top of the distillation tower 5 is recovered and circulated into the solvent storage tank 81. The crude borneol in the bottom of the tower is transported to the freezing crystallization device through the material transfer pump 13, and the crude borneol is obtained through freezing, crystallization and centrifugation.
[0052] Before the hydrogenation reaction stabilizes, the conversion rate of camphor and the content of borneol in the sample detected by sampling at the lower discharge port of gas-liquid separator 4 should be controlled, the feed flow rate of hydrogen and ethanol camphor solution entering fixed-bed reactor 3 is controlled, the temperature and pressure of the reaction in fixed-bed reactor 3 are regulated, the fixed-bed reactor 3 bottom discharge product is separated by gas and liquid, and the content of borneol can reach 63-68%, isoborneol content is between 30-35%, camphor content is 0.1-0.5%, and yield is 98%-99.9%. After the fixed-bed reactor 3 bottom discharge detects and reaches production requirements, each reaction parameter is fixed, and continuous production is started. Camphor solution and hydrogen mixture of ethanol are continuously added to the fixed-bed reactor 3 from the top feed port of fixed-bed reactor 3, and product is continuously discharged from the bottom discharge port of fixed-bed reactor 3 to form continuous production. The whole production process is transmitted to the computer center by the pressure, temperature and flow sensors of each control point, and continuous production fully automatic control is implemented.
[0053] It is worth noting that the concentration of the liquid solution in the heating batching kettle 83 is 10%-80%, the preheating temperature of the liquid preheater 7 is 60℃-180℃, the preheating temperature in the gas preheater 9 is 100℃-200℃, and the gas flow rate of the fixed bed reactor 3 is 800m 3 / h-1000m 3 / h, liquid phase flow rate is 0.1m 3 / h-0.5m 3 / h, the gas-liquid ratio is 1600-10000, the reaction temperature in the fixed bed reactor 3 is 120°C-200°C, and the reaction pressure is 1MPa-5MPa.
[0054] Example 1: First, 1000 kg of granular solid catalyst was loaded into the fixed bed reactor 3, and nitrogen was used to replace the reactor until the reactor was absolutely oxygen-free. Then, hydrogen was preheated by the gas phase preheater 9 and then transported into the fixed bed reactor 3 from the upper inlet. Then, the heating jacket of the fixed bed reactor 3 was opened, and the loaded catalyst was slowly heated to 160°C. The hydrogen compressor 101 was turned on at 800 m 3 / h-1000m 3 / h standard state meter of hydrogen flow is delivered to the hydrogen preheater to preheat the hydrogen to 100 ° C; at the same time, the feed pump is turned on to feed the raw material ethanol camphor solution (mass fraction of 50%) stored in the solvent storage tank 81 and the camphor storage tank 1 at a rate of 0.2m 3 / h flow rate, sent to the liquid phase preheater 7, the mixed solution is heated to 100 ° C; then the preheated hydrogen and ethanol camphor solution are transported to the gas-liquid mixer 6 and mixed evenly, the gas-liquid volume ratio is controlled to 5000, the mixed gas and liquid materials are simultaneously transported to the fixed bed reactor 3, and the hydrogenation reaction is completed at a temperature of 120 ° C and a pressure of 1 MPa; the qualified product coming out of the lower part of the fixed bed reactor 3 is cooled to room temperature through a cooler; the reaction product mixture after cooling enters the gas-liquid separator 4, and the material separated by the gas-liquid separator 4 enters the intermediate storage tank 12, and then is transported to the continuous distillation tower 5 by a pump, and the top of the distillation tower 5 is extracted The solvent is recovered to the solvent storage tank 81, and the concentrated material at the bottom is transported to the crystallization and centrifugation device through the transfer pump 13 to obtain crude borneol, of which borneol is 63.01%, isoborneol is 35.86%, and camphor is 0.58%, and the camphor conversion rate reaches 98.8%; the hydrogen separated by the gas-liquid separator 4 is recycled by the circulating gas compressor 102 and combined with the newly replenished hydrogen and transported to the gas phase preheater 9 again for continuous hydrogenation. The ethanol camphor solution is continuously added from the top feed port of the fixed bed reactor 3, and after mixing with the hydrogen, it directly enters the fixed bed reactor 3. The crude borneol after the hydrogenation reaction is continuously discharged from the end of the reactor to form continuous production.
[0055] Example 2: The hydrogenation reaction temperature was controlled at 120°C, the hydrogenation reaction pressure was set to 2 MPa, and other conditions remained unchanged and the steps of Example 1 were repeated;
[0056] The crude borneol contained 64.76% borneol, 33.21% isoborneol, and 1.58% camphor, with a camphor conversion rate of 97.97%.
[0057] Example 3: The hydrogenation reaction temperature was controlled at 160° C., the hydrogenation reaction pressure was set to 2 MPa, and other conditions remained unchanged and the steps of Example 1 were repeated;
[0058] The crude borneol contained 66.65% borneol, 32.01% isoborneol, and 0.42% camphor, with a camphor conversion rate of 98.66%.
[0059] Example 4: The hydrogenation reaction temperature was controlled at 160° C., the hydrogenation reaction pressure was set to 5 MPa, and other conditions remained unchanged and the steps of Example 1 were repeated;
[0060] The crude borneol contained 68.65% borneol, 31.22% isoborneol, and 0.03% camphor, with a camphor conversion rate of 99.90%.
[0061] Example 5: The hydrogenation reaction temperature was controlled at 160° C., the hydrogenation reaction pressure was set to 5 MPa, the camphor content in the ethanol camphor solution was increased to 80%, and the other conditions remained unchanged and the steps of Example 1 were repeated;
[0062] The crude borneol contained 68.56% borneol, 31.02% isoborneol, and 0.13% camphor, with a camphor conversion rate of 99.58%.
[0063] Example 6: The hydrogenation reaction temperature was controlled at 160° C., the hydrogenation reaction pressure was set to 5 MPa, the camphor content in the ethanol camphor solution was increased to 80%, and the other conditions remained unchanged and the steps of Example 1 were repeated;
[0064] The crude borneol contained 68.56% borneol, 31.02% isoborneol, and 0.13% camphor, with a camphor conversion rate of 99.58%.
[0065] Example 7: The hydrogenation reaction temperature was controlled at 160°C, the hydrogenation reaction pressure was set to 5 MPa, the reaction solvent was changed to dioxane containing 80% camphor, and the other conditions were unchanged and the steps of Example 1 were repeated;
[0066] The crude borneol contained 68.86% borneol, 30.02% isoborneol and 0.21% camphor, and the camphor conversion rate reached 98.88%.
[0067] In summary, the continuous production method of synthesizing borneol from camphor based on a continuous production device directly uses camphor as raw material, and through continuous hydrogenation, concentration, crystallization, and centrifugation, high-quality crude borneol can be obtained. This process method has a short production cycle, a low risk factor, and is harmless to the environment. In addition, the process is simple to operate and has few reaction steps, which solves the problem of computer automation control throughout the production process.
[0068] In addition, the fixed-bed reactor 3 continuous hydrogenation production device and method improves the unstable state in hydrogenation production and effectively improves production efficiency. Therefore, it is convenient to adopt an automatic control system in the production process, greatly reducing the product process instability caused by human operation deviation, so that the hydrogenation production process can meet the requirements of stable product quality, safety, high efficiency and low consumption.
Claims
1. A continuous production device for synthesizing borneol from camphor, comprising a camphor storage tank (1), a hydrogen storage tank (2), a fixed bed reactor (3), a gas-liquid separator (4) and a distillation tower (5), characterized in that: Also includes: a gas-liquid mixer (6), wherein the output end of the gas-liquid mixer (6) is connected to the input end of the fixed bed reactor (3); the liquid phase input end of the gas-liquid mixer (6) is connected to a liquid phase preheater (7); a liquid phase circulation and delivery component (8) is provided between the camphor storage tank (1), the liquid phase preheater (7) and the distillation tower (5); the gas phase input end of the gas-liquid mixer (6) is connected to a gas phase preheater (9); and a gas phase circulation and delivery component (10) is provided between the hydrogen storage tank (2), the gas phase preheater (9) and the gas-liquid separator (4); a condenser (11), the condenser (11) being arranged between the fixed bed reactor (3) and the gas-liquid separator (4), the input end of the condenser (11) being connected to the output end of the fixed bed reactor (3), and the output end of the condenser (11) being connected to the input end of the gas-liquid separator (4); an intermediate storage tank (12), the intermediate storage tank (12) being arranged between the gas-liquid separator (4) and the distillation tower (5), the input end of the intermediate storage tank (12) being connected to the output end of the gas-liquid separator (4), and the output end of the intermediate storage tank (12) being connected to the input end of the distillation tower (5); a material transfer pump (13), the material transfer pump (13) being connected to the output end of the tower kettle of the distillation tower (5); The liquid phase circulation conveying component (8) comprises: a solvent storage tank (81), wherein the input end of the solvent storage tank (81) is connected to the liquid phase output end of the distillation tower (5); the output end of the solvent storage tank (81) is connected to a solvent delivery pump (82); the output end of the solvent delivery pump (82) and the output end of the camphor storage tank (1) are connected to a heating and dispensing kettle (83); and the output end of the heating and dispensing kettle (83) is connected to a liquid phase delivery pump (84); a liquid flow meter (85), wherein the input end of the liquid flow meter (85) is connected to the output end of the liquid phase delivery pump (84), and the output end of the liquid flow meter (85) is connected to the input end of the liquid phase preheater (7); The gas phase circulation conveying component (10) comprises: a hydrogen compressor (101), wherein the input end of the hydrogen compressor (101) is connected to the output end of the hydrogen storage tank (2); A circulating gas compressor (102), wherein the input end of the circulating gas compressor (102) is connected to the gas phase output end of the gas-liquid separator (4), the output end of the circulating gas compressor (102) and the output end of the hydrogen compressor (101) are commonly connected to a gas flow meter (103), and the output end of the gas flow meter (103) is connected to the input end of the gas phase preheater (9).
2. A production method using the continuous production device for synthesizing borneol from camphor according to claim 1, characterized in that: The continuous production method of borneol synthesized from camphor is based on a continuous production device and comprises the following steps: S1, camphor hydrogenation reaction: first, the catalyst is loaded into a heated pressure-resistant fixed-bed reactor (3), and nitrogen is used for replacement to ensure that the device is absolutely oxygen-free, then the fixed-bed reactor (3) heating device is turned on, and the temperature of the fixed-bed reactor (3) is maintained under reaction conditions, the camphor solution enters the liquid phase circulation conveying component (8) from the camphor storage tank (1) for batching and dissolution, and is sent to the liquid phase preheater (7) for preheating treatment, while hydrogen enters the gas phase circulation conveying component (10) from the hydrogen storage tank (2) for compression and is sent to the gas phase preheater (9) for preheating treatment, and is sent together to the gas-liquid mixer (6) for uniform mixing, and finally is sent from the upper part of the fixed bed reactor (3) into the fixed bed reactor (3) for hydrogenation reaction; S2, gas-liquid separation: the material coming out of the end of the fixed bed reactor (3) in step S1 enters the condenser (11), and then enters the gas-liquid separator (4) for gas-liquid separation. The separated hydrogen is transported by the gas phase compressor and combined with the new hydrogen sent by the hydrogen compressor (101), and then preheated by the gas phase preheater (9), enters the gas-liquid mixer (6) and is mixed with the ethanol camphor solution from the liquid phase preheater (7), and then returns to the fixed bed reactor (3) for cyclic hydrogenation reaction; S3, distillation separation: The material subjected to gas-liquid separation in the gas-liquid separator (4) in step S2 reaches the intermediate storage tank (12) and then enters the continuous distillation tower (5) for separation. Most of the reaction solvent at the top of the distillation tower (5) is recovered and circulated into the solvent storage tank (81). The crude borneol in the bottom of the tower is transported to the freezing crystallization device through the material transfer pump (13). After freezing, crystallization, and centrifugation, the crude borneol product is obtained.
3. The method for continuously producing borneol from camphor according to claim 2, wherein: The concentration of the liquid solution in the heating batching kettle (83) is 10%-80%, and the preheating temperature of the liquid preheater (7) is 60°C-180°C.
4. The method for continuously producing borneol from camphor according to claim 3, wherein: The preheating temperature in the gas phase preheater (9) is 100°C-200°C.
5. The method for continuously producing borneol from camphor according to claim 4, characterized in that: The gas phase flow rate of the fixed bed reactor (3) is 800m 3 / h-1000m 3 / h, liquid phase flow rate is 0.1m 3 / h-0.5m 3 / h, gas-liquid ratio is 1600-10000.
6. The method for continuously producing borneol from camphor according to claim 5, characterized in that: The reaction temperature in the fixed bed reactor (3) is 120°C-200°C, and the reaction pressure is 1MPa-5MPa.
Citation Information
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