Process for the synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor
By using a gas-liquid two-phase flow disperser in a supergravity reactor to enhance the interphase mass transfer process between the gas and liquid phases, the problems of easy clogging in microchannel reactors and long material residence time in traditional batch reactors were solved, achieving efficient synthesis of 2-chloro-2-oxo-1,3,2-dioxophosphazenecyclopentane, and improving yield and product quality.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NANKAI UNIV
- Filing Date
- 2023-07-12
- Publication Date
- 2026-04-10
AI Technical Summary
In existing technologies, microchannel reactors are prone to clogging, have insufficient gas-liquid mixing, and slow oxidation rates. Furthermore, traditional batch reactors have long material residence times and produce many byproducts, resulting in low yields and insufficient production capacity of 2-chloro-2-oxo-1,3,2-dioxophosphazenecyclopentane.
A supergravity reactor is used, and a gas-liquid two-phase flow disperser is designed to form highly dispersed microdroplets when the gas and liquid materials enter the reactor. These microdroplets then form nanoscale liquid films and droplets in the centrifugal field of the high-speed rotating rotor, thereby enhancing the interphase mass transfer process between the gas and liquid phases and improving the oxidation reaction efficiency.
It significantly improves gas-liquid mass transfer efficiency and heat exchange efficiency, shortens reaction time, increases reaction conversion rate and product yield, reduces by-products, and results in high product quality.
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Figure CN117085617B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of organic synthesis and chemical production, in particular to a method for synthesizing 2-chloro-2-oxo-1,3,2-dioxaphospholane by using a supergravity reactor. BACKGROUND
[0002] With the continuous development of society, people's demand for life quality and industrial products is increasing, and the demand for biocompatible and affinity products continues to grow. The organic compound 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP) is an important chemical intermediate, which belongs to the phosphorus oxychloride compound, which is widely used in the synthesis of pesticides, antibiotics, fungicides, retardants, lubricants, flame retardants, cosmetics and other substances, and it is also an important intermediate for synthesizing various bioactive compounds such as aminophosphates, phosphonates, enol phosphates, and diamine phosphates. In addition, such phosphorus oxychloride compounds are also important intermediates for synthesizing anticoagulant materials, blood compatible materials, biocompatible materials, drug controlled release systems, phosphocholine drugs, high-end cosmetics, and biologically friendly surfactants, and are also key raw materials for preparing 2-methacryloyloxyethyl phosphocholine, with a very broad application prospect.
[0003] 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP) is traditionally prepared by using phosphorus trichloride and ethylene glycol as raw materials, dichloromethane as a solvent, and dropping in a kettle reactor under temperature control to synthesize 2-chloro-1,3,2-dioxaphospholane (CUP); then CUP is purified by vacuum distillation technology and dissolved in toluene, and then dry air, oxygen or ozone is introduced into the kettle reactor under back pressure to oxidize CUP to 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP), but the reaction yield is very low, the reaction time needs to be prolonged to improve the yield, and the reaction time is usually 48h-7d, so that the production capacity is very low. Moreover, the conventional kettle oxidation process has a long residence time of materials, many by-products, and often has a gel phenomenon due to long-time reaction, which affects the long-term operation of the reaction device. Chinese patent CN106946936A introduces dry oxygen and 2-chloro-1,3,2-dioxaphospholane into a microchannel reactor for gas-liquid reaction to realize online synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP), but this patent still has some deficiencies, that is, the gas-liquid mixing efficiency is not high enough, the oxidation speed is not fast enough, and with the prolongation of the reaction time, gel will block the microchannel reactor during the reaction, which increases the difficulty of subsequent maintenance, and the microchannel reactor device has relatively high investment, the operation difficulty is also relatively large, and the control system requirement is relatively high, which still needs to accumulate more production experience. Therefore, it is urgent to use a fast and efficient synthesis method for preparing 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP), especially to solve the problem of easy plugging of the microchannel reactor.
[0004] The reactor is the main place where chemical reactions occur. Common reactor types include fluidized bed reactors, fixed bed reactors, stirred tank reactors, and microchannel reactors. Common reaction types include gas-liquid, liquid-liquid, gas-solid, gas-liquid-solid, and other multiphase reactions. In the gas-liquid reaction type, the most commonly used reactor in industry is the fixed bed reactor or the fluidized bed reactor, which is to load the catalyst in the fixed bed layer or maintain fluidization in the fluidized bed, and carry out gas-liquid-solid phase catalytic reaction under certain temperature and pressure. However, the fixed bed has the problems of large pressure drop, uneven bed temperature distribution, complex structure of the fluidized bed, serious catalyst wear, and other problems, and the catalytic hydrogenation reaction process is difficult to control well, which affects the catalytic effect, and at the same time, such equipment also has the problems of large occupied area, high industrial energy consumption, etc.
[0005] In recent years, supergravity technology has made important progress in the application research in chemical industry, such as CN103102942A successfully puts the raw oil into the supergravity reactor loaded with non-noble metal catalyst, and contacts with hydrogen in countercurrent to carry out desulfurization, denitrification and partial aromatic saturation reaction; CN107540555A disperses hydrogen into a large number of nanometer bubbles in the organic compound containing nitro group in the supergravity reactor, and carries out gas-liquid-solid catalytic hydrogenation reaction process on the surface of the regular packing loaded with metal catalyst. The reactor used in the method can make the solubility of the difficultly soluble hydrogen in the liquid phase reach supersaturation, efficiently utilize the reducing hydrogen, and strengthen the gas-liquid-solid phase mass transfer, so that good gas-liquid reaction effect is achieved. The supergravity reactor has a wide potential value in the application in gas-liquid reaction.
[0006] However, the current feeding mode of the supergravity reactor is to separately feed the liquid and the gas, and the gas-liquid is dispersed into nanometer gas-liquid bubbles by the supergravity generated by the high-speed rotation of the rotor after the mixing in the feeding cavity. The mixing mode has a certain hysteresis, and the gas-liquid dispersion effect is affected. SUMMARY
[0007] The technical problem to be solved by the present application is to provide a method for synthesizing 2-chloro-2-oxygen-1,3,2-dioxaphospholane by using a supergravity reactor. The method changes the traditional supergravity reactor gas-liquid material separate feeding mode, and uses a gas-liquid two-phase flow disperser to form high-dispersibility microdroplets with a particle size of 10 microns when the gas-liquid material enters the supergravity reactor. The microdroplets are subjected to a large shear force in the strong centrifugal field generated by the high-speed rotation of the rotor to form nanoscale liquid membranes, droplets, and generate rapidly updated phase interfaces. The interphase mass transfer process of the gas-liquid two-phase in the high dispersion and strong turbulent flow is strengthened, so that the oxidation reaction effect of 2-chloro-1,3,2-dioxaphospholane is improved, and the reaction rate is accelerated.
[0008] To solve the above technical problems, the application adopts the following technical scheme: a method for synthesizing 2-chloro-2-oxygen-1,3,2-dioxaphospholane by using a supergravity reactor, which is realized by the following method:
[0009] The high gravity reactor comprises a high-speed motor, a main shaft, a rotor, a jacketed shell and an ultrasonic two-phase flow disperser; the main shaft at the output end of the high-speed motor penetrates through the bottom of the jacketed shell and extends into the jacketed shell; the rotor is fixed on the upper part of the main shaft; the ultrasonic two-phase flow disperser is arranged in the jacketed shell, and six ultrasonic two-phase flow dispersers are uniformly distributed in the jacketed shell at equal intervals on each side, and the injection ports of the ultrasonic two-phase flow dispersers face the rotor, and the injection ports spray the gas-liquid mixture at high speed on the inner edge of the rotor; the ultrasonic two-phase flow disperser is provided with a gas inlet and a liquid inlet for inputting oxygen and 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid into the ultrasonic two-phase flow disperser respectively; the lower part of the jacketed shell is provided with a liquid phase outlet; the upper part of the jacketed shell is provided with a gas outlet with a back pressure valve, and the side of the jacketed shell is further provided with a second gas inlet.
[0010] In the application, oxygen is introduced into the outer cavity of the rotor by the gas inlet of the ultrasonic two-phase flow disperser, and is rapidly mixed and reacted with the gas-liquid mixture on the inner edge of the rotor under the action of gas pressure. The gas-liquid mixture entering the rotor is affected by the high-speed rotor, the circumferential speed increases, a higher centrifugal force is generated, and the gas-liquid mixture is pushed to the outer edge of the rotor. In this process, the liquid is dispersed and broken to form a large and constantly updated surface area, and the tortuous flow channel generated by the high-speed rotation of the rotor intensifies the renewal of the gas-liquid surface; in addition, the oxygen introduced tangentially from the second gas inlet collides and mixes with the gas-liquid mixture pushed to the outer edge of the rotor by the high-speed rotor, so that excellent mass transfer and reaction conditions are formed in the rotor. The liquid is thrown by the rotor to the shell and then leaves the high gravity machine through the liquid phase outlet. Oxygen leaves the rotor from the center of the rotor and is introduced out of the rotor through the gas outlet with a back pressure valve, and the mass transfer and reaction process is completed.
[0011] The high-speed motor of the high gravity reactor is started to drive the rotor to rotate at high speed, and oxygen and 2-chloro-1,3,2-dioxaphospholane (CUP) reaction liquid are input into the ultrasonic two-phase flow disperser for high-efficiency gas-liquid two-phase mixing, and the gas-liquid mixture is sprayed onto the rotor;
[0012] The strong centrifugal force generated by the high-speed rotation of the rotor makes the oxygen and 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid receive a huge shearing force in the centrifugal field to form nanoscale liquid film, liquid droplets, and rapidly updated phase interface, and the interphase mass transfer process of the gas-liquid two-phase in the high dispersion and strong turbulent flow is intensified. Under the action of gas pressure and high gravity, oxygen is dispersed into a large amount of nanometer gas bubbles in the CUP reaction liquid, and the solubility of oxygen in the CUP reaction liquid reaches supersaturation, and the CUP rapidly reacts on the surface of the nanometer gas bubbles to complete the gas-liquid two-phase oxidation reaction process to obtain COP.
[0013] The above reaction product and unreacted oxygen are further removed from the reactor through liquid phase sampling outlet and gas outlet with back pressure valve respectively, the product is reduced to room temperature through condenser, and then enters the gas-liquid separation tank, oxygen is sampled from the upper part, and the liquid phase product is sampled from the lower part of the separation tank.
[0014] As a further improvement of the technical solution, the entire reaction system device is first purged with high-purity oxygen to replace the air and water vapor inside the system device, so that the system is in a high-dry state and the system pressure is stable.
[0015] As a further improvement of the technical solution, the ultrasonic two-phase flow disperser is arranged at the upper part of the jacketed shell, the lower end thereof extends into the jacketed shell, and the ultrasonic two-phase flow disperser jet port is opposite to the rotor; the ultrasonic two-phase flow disperser is provided with a gas inlet and a liquid inlet; the ultrasonic two-phase flow disperser is composed of two rows of dispersers, each row of dispersers is composed of six gas-liquid two-phase flow atomizers; and the ultrasonic two-phase flow disperser can synchronously disperse the gas-liquid material to form highly dispersed microdroplets with a particle size of 10 um.
[0016] As a further improvement of the technical solution, the material of the rotor includes titanium alloy, hastelloy alloy, chromium-based alloy, duplex steel or ceramic, etc.
[0017] As a further improvement of the technical solution, the jacketed shell is a double-layer jacket structure, and the temperature of the shell can be controlled by a high-low temperature all-in-one machine.
[0018] As a further improvement of the technical solution, the preparation method of the 2-chloro-1,3,2-dioxaphospholane CUP reaction solution is to dissolve CUP into a solvent to prepare a mixed solution, the solvent is one or more of benzene, toluene and cyclohexane, the volume ratio of CUP to the solvent is 1:2-5, preferably the volume ratio of CUP to the solvent is 1:3-4.
[0019] As a further improvement of the technical solution, the effective gas-liquid mixing ratio of oxygen and 2-chloro-1,3,2-dioxaphospholane input into the ultrasonic two-phase flow disperser is 5%-95%.
[0020] As a further improvement of the technical solution, the size of the nanometer and micrometer bubbles of oxygen dispersed in the CUP reaction solution is controlled to be 50 nm-5 um.
[0021] As a further improvement of the technical solution, the internal operating pressure of the supergravity reactor is controlled to be 0.1-3.0 MPa, and the reaction temperature is controlled to be 0-85℃; preferably, the temperature is controlled to be 10-60℃, and the pressure is controlled to be 0.15-1.5 MPa; more preferably, the CUP oxidation reaction temperature is controlled to be 15-50℃, and the pressure is controlled to be 0.2-0.4 MPa.
[0022] As a further improvement to the technical solution, the residence time of the gas-liquid oxidation reaction is controlled by adjusting the rotation speed of the centrifugal reactor. The rotation speed of the centrifugal reactor can be controlled between 200-4000 rpm, and the residence time of the gas and liquid phases in the rotor can be controlled between 50-2000 ms. Preferably, when the rotor speed is 200 rpm, the residence time is approximately 2000 ms; when the rotor speed is 1000 rpm, the residence time is approximately 800 ms; when the rotor speed is 2000 rpm, the residence time is approximately 100 ms; and when the rotor speed is 4000 rpm, the residence time is approximately 50 ms.
[0023] When the residence time in a single-pass reaction is short, the conversion rate of the oxidation reaction is low. This conversion rate can be improved by external material circulation. By adjusting the rotational speed of the centrifugal reactor, the molecular mixing efficiency and material residence time can be controlled, thereby improving the efficiency of the CUP oxidation reaction.
[0024] Unless otherwise specified, all raw materials used in this invention can be obtained commercially, and the equipment used in this invention can be conventional equipment in the relevant field or refer to existing technology in the relevant field.
[0025] Compared with the prior art, the present invention has the following beneficial effects:
[0026] 1) High gas-liquid mass transfer efficiency significantly improves heat exchange efficiency. The ultrasonic two-phase flow disperser can efficiently mix gas and liquid to generate 10µm microdroplets. When the bubble diameter is less than 50µm, the surface tension at the microbubble interface has a significant impact on bubble characteristics. This surface tension compresses the internal gas, causing the microbubbles to continuously contract and self-pressurize as they rise. As the bubble diameter shrinks infinitely, the specific surface area of the bubble interface also increases infinitely, eventually leading to an infinitely high internal pressure due to the self-pressurization effect. Therefore, more gas passes through the gas-liquid interface and dissolves into the solvent, continuously enhancing the mass transfer efficiency at the gas-liquid interface. This characteristic allows the microbubbles to continue the gas mass transfer process and maintain high efficiency even when the gas content in the liquid phase reaches supersaturation. The reaction and gas dissolution occur simultaneously. While the gaseous reactants are consumed, the dissolution of nano- and micro-bubbles and the macro-gas phase mass transfer and dissolution into the liquid phase occur concurrently, allowing for immediate gas replenishment. Furthermore, the numerous nano- and micro-bubbles and CUP reactions accelerate heat exchange within the system, resulting in a high heat exchange rate. This facilitates the removal of exothermic reactions, preventing prolonged heating and heat-sensitive denaturation of materials, and reducing the generation of byproducts. Consequently, this process results in fewer side reactions, lighter product color, and higher product quality. The gas-liquid mass transfer rate is 1-3 orders of magnitude higher than that of batch reactions, increasing the yield from 50% to 95%, and shortening the reaction time from 48 hours to 5 minutes.
[0027] 2) The residence time of the bubbles in the liquid phase can be controlled to be prolonged, and the reaction conversion rate is improved. In a common gas-liquid mixing device, the bubbles will quickly rise to the surface of the liquid phase and break and disappear, and the residence time is very short. The gas-liquid two phases can be mixed efficiently by the supergravity reactor of the application, thereby generating a large number of nanometer and micrometer bubbles. Due to the small size effect and the interface effect, the rising speed of the bubbles in the reaction system is very slow, and the process from generation to breakage usually takes tens of seconds or even minutes. Moreover, the volume of the bubbles is continuously contracted and dissolved and disappears in the solvent in the rising process, and the smaller the volume of the bubbles, the slower the rising speed of the bubbles in the solvent. The selection of benzene, toluene and cyclohexane solvents further increases the solvation effect and improves the solubility of oxygen in the reaction system, thereby greatly improving the reaction conversion rate.
[0028] 3) The supergravity reactor of the application has a high-efficiency gas-liquid mixing effect, and the oxygen content in the liquid phase can be as high as 95%. The nanometer and micrometer bubbles are broken in the liquid phase to generate cavitation shear force, which promotes the CUP oxidation reaction. At the same time, under the action of supergravity, the gas phase can be redissolved, so that the gas-liquid two-phase reaction can be carried out efficiently under low pressure (0.4 Mpa), thereby greatly improving the safety of the reaction. BRIEF DESCRIPTION OF DRAWINGS
[0029] Figure 1 The supergravity reactor of the application is shown in the schematic diagram.
[0030] Wherein: 1-liquid storage tank; 2-liquid feeding pump; 3-liquid flow meter; 4-high pressure oxygen cylinder; 5-gas flow meter; 6-ultrasonic two-phase flow disperser; 7-rotor; 8-main shaft; 9-high-speed motor; 10-back pressure valve; 11-shell with jacket; 12-liquid phase sampling outlet; 13-second gas inlet; 14-condenser; 15-gas-liquid separation tank; DETAILED DESCRIPTION
[0031] The treatment method of the application will be described in detail below in combination with examples.
[0032] The application provides a method for synthesizing 2-chloro-2-oxygen-1,3,2-dioxaphospholane in a high gravity reactor, wherein the high gravity reactor comprises a high-speed motor 9, a main shaft 8, a rotor 7, a jacketed shell 11 and an ultrasonic two-phase flow disperser 6, the output end of the high-speed motor 9 is connected with the main shaft 8 which penetrates through the bottom of the jacketed shell 11 and extends into the jacketed shell 11, the rotor 7 is fixed on the upper part of the main shaft 8, the ultrasonic two-phase flow disperser 6 is arranged in the jacketed shell 11 and the jetting port of the ultrasonic two-phase flow disperser 6 is opposite to the rotor 7, the ultrasonic two-phase flow disperser 6 is provided with a gas inlet and a liquid inlet for inputting oxygen and 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid into the ultrasonic two-phase flow disperser respectively, the lower part of the jacketed shell 11 is provided with a liquid phase outlet 12, the upper part of the jacketed shell 11 is provided with a gas outlet with a back pressure valve 10, and the side of the jacketed shell 11 is further provided with a second gas inlet 13.
[0033] In the method, the ultrasonic two-phase flow disperser 6 performs high-efficiency mixing of oxygen and 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid in gas-liquid two phases, sprays the gas-liquid mixture onto the rotor 7, utilizes the strong centrifugal force generated by the high-speed rotation of the rotor 7, and forms nanoscale liquid film and liquid drops and generates rapidly updated phase interface by the great shearing force of the liquid and gas in the centrifugal field, so that the gas-liquid two-phase interfacial mass transfer process in high dispersion and strong turbulence is strengthened, the oxygen is dispersed into a large number of nanometer oxygen bubbles in the CUP reaction liquid, the solubility of the oxygen in the CUP reaction liquid reaches supersaturation, the CUP rapidly reacts on the surface of the nanometer oxygen bubbles, the gas-liquid two-phase oxidation reaction process is completed, and the product COP is obtained. The obtained product is further reduced to room temperature through the condenser 14, then enters the gas-liquid separation tank 15, the oxygen is taken out from the upper part, and the liquid phase product is taken out from the lower part of the separation tank.
[0034] Example 1
[0035] 2-chloro-1,3,2-dioxaphospholane (CUP) and cyclohexane are mixed into a reaction liquid with a volume ratio of 1:3 and are added into a liquid storage tank 1. The temperature of the high gravity reactor is controlled at 20℃, the rotating speed is adjusted to 2000r / min, the solution in the liquid storage tank 1 is continuously pumped into the high gravity reactor at a flow rate of 200mL / min through a liquid feeding pump 2, high-purity oxygen in a high-pressure oxygen cylinder 4 is continuously introduced into the high gravity reactor at a speed of 50L / min, the system back pressure is 0.3Mpa, the gas-liquid volume ratio is 250:1, and the gas-liquid countercurrent reaction is carried out, the reaction residence time is about 5min, then the mixed slurry is pumped into a molecular distillation device, and clear and transparent 2-chloro-2-oxygen-1,3,2-dioxaphospholane (COP) is obtained by vacuum distillation under the conditions of temperature control of 90℃ and absolute pressure of 20pa, and the yield is 96.1%.
[0036] Example 2:
[0037] The operating conditions are the same as in Example 1, except that the solvent cyclohexane is replaced by toluene, the volume ratio of CUP to toluene is 1:4, the temperature of the high gravity reactor is controlled at 25°C, and the final product is a clear transparent colorless sample with a yield of 95.5%.
[0038] Example 3:
[0039] The operating conditions are the same as in Example 1, except that the temperature of the high gravity reactor is controlled at 35°C and the rotation speed is adjusted to 4000 r / min, and the final product is a clear transparent colorless sample with a yield of 96.3%.
[0040] Example 4:
[0041] The operating conditions are the same as in Example 1, except that the solvent is replaced by benzene, the volume ratio of CUP to benzene is 1:4, the oxygen flow rate is 80 L / min, the temperature is controlled at 25°C, the rotation speed is 4000 r / min, the system back pressure is 0.2 MPa, and the gas-liquid volume ratio is 400:1, and the final product is a clear transparent colorless sample with a yield of 97.0%.
[0042] Comparative Example 5:
[0043] A reaction system with a volume ratio of CUP (molar mass of 50 mol) to toluene of 1:4 is prepared and added to a reaction kettle. In order to improve the reaction efficiency, the temperature of the reaction kettle is controlled at 50°C, and the reaction kettle is slowly aerated with a titanium alloy aeration head, with a gas flow rate of 500 mL / min, a reaction kettle back pressure of 0.3 MPa, and stirring for 48 h. A 200 g sample is then taken out for yield determination, and the purification conditions for molecular distillation are: temperature control at 90°C, absolute pressure of 20 Pa, and vacuum distillation to obtain a clear transparent 2-chloro-2-oxy-1,3,2-dioxaphospholane (COP) with a yield of 46.6%.
[0044] As can be seen from the above examples, the present application has higher reaction efficiency, shorter reaction time, and higher product yield than the kettle process. The above is only a preferred embodiment of the present application, enabling those skilled in the art to understand or implement the present application. Various modifications and combinations of these examples will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these examples shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A process for the synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor, characterized in that, The supergravity reactor comprises a high-speed motor, a main shaft, a rotor, a jacketed shell and an ultrasonic two-phase flow disperser; the main shaft at the output end of the high-speed motor penetrates through the bottom of the jacketed shell and extends into the jacketed shell; the rotor is fixed on the upper part of the main shaft; the ultrasonic two-phase flow disperser is arranged in the jacketed shell, and the jet port of the ultrasonic two-phase flow disperser faces the rotor; the ultrasonic two-phase flow disperser is provided with a gas inlet and a liquid inlet; the lower part of the shell is provided with a gas-liquid outlet; the upper part of the jacketed shell is provided with a gas outlet with a back pressure valve, and the side of the jacketed shell is further provided with a second gas inlet; the method is as follows: Start the high-speed motor of the supergravity reactor to drive the rotor to rotate at high speed, and input oxygen and 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid into the ultrasonic two-phase flow disperser for high-efficiency mixing of gas-liquid two phases, and spray the gas-liquid mixture onto the rotor; The strong centrifugal force generated by the high-speed rotation of the rotor makes the oxygen and the 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid receive a huge shearing force in the centrifugal field to form nanoscale liquid film, liquid droplets, and a rapidly updated phase interface, and the interphase mass transfer process of the gas-liquid two phases in the high dispersion and strong turbulent flow is strengthened, under the action of gas pressure and supergravity, the oxygen is dispersed into a large amount of nanometer oxygen bubbles in the CUP reaction liquid, and the solubility of the oxygen in the CUP reaction liquid reaches supersaturation, the CUP rapidly reacts on the surface of the nanometer oxygen bubble to complete the gas-liquid two-phase oxidation reaction process to obtain COP.
2. A process for the synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein Further comprising the following steps: The oxygen is tangentially input into the jacketed shell from the second gas inlet, and the input oxygen collides and mixes with the gas-liquid mixture pushed by the high-speed rotor to the outer edge of the rotor to form a mass transfer and reaction condition in the rotor.
3. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The ultrasonic two-phase flow disperser is arranged on the upper part of the jacketed shell, and the lower end thereof extends into the jacketed shell, the ultrasonic two-phase flow disperser is composed of two rows of dispersers, each row of dispersers is composed of six gas-liquid two-phase flow atomizers, and the ultrasonic two-phase flow disperser synchronously disperses the gas-liquid materials.
4. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The 2-chloro-1,3,2-dioxaphospholane CUP reaction liquid comprises CUP and a solvent, the reactant is CUP, and the solvent is one or more of benzene, toluene or cyclohexane; the volume ratio of CUP to the solvent is 1:2-5.
5. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The gas-liquid mixing ratio of the oxygen and the 2-chloro-1,3,2-dioxaphospholane input into the ultrasonic two-phase flow disperser is 5%-95%. The rotation speed of the supergravity reactor is 200-4000 r / min.
6. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1 or 5 wherein: The rotation speed of the supergravity reactor is 1500-3000 r / min.
7. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The size of the nanometer oxygen bubbles dispersed in the CUP reaction liquid is controlled to be 50 nm-5 μm.
8. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The temperature of the rapid reaction of CUP on the surface of the nanometer oxygen bubble is 0-85 ℃, the pressure is 0.1-3.0 MPa, and the gas-liquid volume ratio is 25:1-1000:
1.
9. The process for synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane in a high gravity reactor as claimed in claim 1, wherein: The temperature of the rapid reaction of CUP on the surface of the nanometer oxygen bubble is 10-60 ℃, the pressure is 0.15-1.5 MPa, and the gas-liquid volume ratio is 30:1-800:
1.
10. A method for synthesizing 2-chloro-2-oxo-1,3,2-dioxophosphazenecyclopentane in a supergravity reactor according to claim 1, 8, or 9, characterized in that: The temperature for the fast reaction of CUP on the surface of nano-micro oxygen bubbles is 15-50 ℃, the pressure is 0.2-0.4 MPa, and the gas-liquid volume ratio is 50:1-400:1.
Citation Information
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