Industrial control method and system for perfluoropolyether acyl fluoride

By adopting the screw ring structure of external ultraviolet light source and photosynthetic reaction equipment in the industrial control system of perfluoropolyetherfluoride, the light efficiency fluctuation and reaction out-of-control problems caused by UV light source contacting reaction materials in traditional reactors are solved, and efficient and stable photooxidation polymerization reaction is achieved, which is suitable for large-scale industrial production.

CN119346038BActive Publication Date: 2025-03-25CHENGDU CHENGUANG BODA RUBBER PLASTIC CO LTD +1
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Patent Information

Application Number
CN202411898283.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-23
Publication Date
2025-03-25
Estimated Expiration
2044-12-23

AI Technical Summary

Technical Problem

In the prior art, the UV light source directly contacts the reaction material and product in the reactor, resulting in fluctuations in the light efficiency and affects the stability of the reaction. In addition, traditional kettle reactors have problems of out-of-control and safety risks.

Method used

The external ultraviolet light source is arranged, and the spray flows into the screw ring in the photosynthesis reaction equipment, moves upward along the screw ring and reacts under the action of the ultraviolet lamp and the heat exchange column. The continuous photooxidation polymerization reaction control is achieved by controlling the power and temperature of the ultraviolet lamp.

Benefits of technology

It shortens the reaction time, improves the reaction efficiency, improves the stability and operability of the reaction system, is suitable for large-scale industrial production, and improves product quality.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses an industrial control method and system for perfluoropolyether acyl fluoride, which belongs to the field of fluorine chemical technology. An external ultraviolet light source is used to avoid direct contact between the light source and the reaction materials. Unlike the traditional kettle reactor, which often causes corrosion because the light source must be arranged in the kettle, affecting the normal reaction and even causing safety risks, the stability and operability of the reaction system can be greatly improved, and it is suitable for large-scale industrial production. Different from the traditional kettle reactor, it is a continuous flow reaction form without material backmixing, and the reaction temperature and reaction residence time are stably controlled, so the product quality can be improved relative to the kettle reaction form.
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Description

Technical Field

[0001] The invention relates to the technical field of fluorine chemical industry, and in particular to an industrial control method and system for perfluoropolyether acyl fluoride. Background Art

[0002] Perfluoropolyether (PFPE) is a high molecular polymer that is an oily liquid at room temperature. Due to its unique thermal stability, oxidation stability, high insulation strength and low toxicity, it can be used as an ideal test liquid for electronic reliability tests, and is used as a thermal shock oil for air tightness tests and hot and cold shock tests in the fields of semiconductors and electronic packaging. In industrial production, perfluoroolefins and oxygen are usually used as raw materials. After polymerization by chemical initiators or ultraviolet light to obtain perfluoropolyether acyl fluoride, stable perfluoropolyether is obtained by fluorination treatment. Therefore, perfluoropolyether acyl fluoride is the precursor for obtaining perfluoropolyether and is also the key to determining the conversion rate of perfluoropolyether.

[0003] The Chinese patent with publication number CN117680071A and publication date 2024.03.12 discloses an industrial control method for the efficient synthesis of perfluoropolyether acyl fluoride, using hexafluoropropylene and oxygen as raw materials, and introducing fluorine fluid to react in a photocatalytic oxidation reactor, wherein an ultraviolet lamp, an agitator and a gas distributor are provided in the photocatalytic oxidation reactor, a liquid feed port, a gas phase outlet and a reflux port are provided at the upper part of the photocatalytic oxidation reactor, a gas feed port and a discharge port are provided at the lower part of the photocatalytic oxidation reactor, a gas distributor is provided on the gas feed port, and the gas distributor is located at the bottom of the photocatalytic oxidation reactor, and various process control parameters of the photocatalytic oxidation reactor are controlled during the reaction. In this patent, the UV light source still adopts a built-in structure, and the light source is in direct contact with the reaction materials and products. Due to corrosion, product contamination, etc., the light efficiency fluctuates with the reaction and affects the reaction stability.

[0004] A Chinese patent with publication number CN116637574A and publication date 2023.08.25 discloses a process system and method for the synthesis of medium and low molecular weight perfluoropolyethers, which includes oxidative polymerization, crude product phase separation, stabilization treatment and distillation separation. The reaction raw materials hexafluoropropylene and fluorine-oxygen mixed gas undergo oxidative polymerization in an oxidative polymerization reactor. The gas is fully discretized by high-speed mechanical shearing and liquid collision mixing, and the reactor is temperature controlled by coupling the integrated heat exchange structure. The phase separator collects the crude perfluoropolyether product, which is preheated and passed into the fluorination reactor for fluorination stabilization treatment. The stabilized perfluoropolyether is passed through a distillation tower to obtain products with different molecular weight distributions. The structure of the reactor in this patent is complex, and fluorine gas is used as a polymerization initiator. Fluorine gas, as a super-reactive substance, has hazards and potential risks such as high heat generation and violent reaction leading to reaction out of control.

[0005] The Chinese patent with publication number CN118546351A and publication date 2024.08.27 discloses a method for preparing perfluoropolyether acyl fluoride by continuous cross-flow photooxidation reaction, wherein hexafluoropropylene at -50~-40℃ is sequentially passed through the photooxidation reactors connected in series and oxygen and chlorotrifluoroethylene gas are introduced from the bottom of each photooxidation reactor to undergo photooxidation reaction under ultraviolet light excitation; the reaction liquid overflowing from the upper side of the last photooxidation reactor directly enters the room temperature hexafluoropropylene evaporation recovery kettle, and the vaporized hexafluoropropylene is condensed and circulated to the hexafluoropropylene raw material storage tank for recycling; the number of photooxidation reactors is ≥2. In this patent, the UV light source is built-in, and the light source is in direct contact with the reaction materials and products. Due to corrosion, product contamination, etc., the light efficiency fluctuates with the reaction and affects the reaction stability; in addition, although the gas phase and liquid phase materials are fed in the form of reverse cross-flow with lower and upper double inlets, due to the huge differences in boiling points and surface energies of oxygen, chlorotrifluoroethylene and hexafluoropropylene, it may not be possible to achieve an efficient gas-liquid dispersion effect. Summary of the invention

[0006] The present invention aims to solve the problems existing in the prior art and provides an industrial control method and system for perfluoropolyether acyl fluoride, which realizes the continuous photo-oxidative polymerization reaction control of ultraviolet light irradiation catalytic reaction of fluorinated olefins under low temperature conditions. Different from the traditional kettle-type intermittent reaction system, the reaction time can be greatly shortened and the reaction efficiency is improved, which is suitable for large-scale industrial production.

[0007] The objective of the present invention is achieved through the following technical solutions:

[0008] An industrial control method for perfluoropolyether acyl fluoride comprises the following steps:

[0009] Step 1, hexafluoropropylene and oxygen flow into the mixer through the hexafluoropropylene inlet pipe and the oxygen inlet pipe respectively, and the material control units on the hexafluoropropylene inlet pipe and the oxygen inlet pipe control the feed amounts of hexafluoropropylene and oxygen, so that the hexafluoropropylene and oxygen are fully mixed in the mixer and atomized into a spray;

[0010] Step 2: The spray is continuously fed into a spiral ring with openings at both ends in the photosynthetic reaction device, and the spray moves upward along the spiral ring, and the spray reacts under the action of the ultraviolet lamp and the heat exchange column; the power of the ultraviolet lamp at the photosynthetic reaction device and the first temperature control unit are controlled to make the spray react in the photosynthetic reaction device to obtain a product liquid;

[0011] Step 3: the product liquid is discharged into the intermediate buffer tank through the product outlet pipe, and finally discharged into the evaporation tank through the third discharge pipe for evaporation to obtain perfluoropolyether acyl fluoride.

[0012] Preferably, the height-to-diameter ratio of the photosynthetic reaction device is 10-20:1.

[0013] Preferably, the flow rate of the hexafluoropropylene inlet pipe is 20-40 Kg / h; the flow rate of the oxygen inlet pipe is 0.5-5 Kg / h.

[0014] Preferably, the power of the ultraviolet lamp is controlled at 1500~3000W, and the first temperature control unit includes a first temperature sensor arranged at the lower part of the transparent jacket, a second temperature sensor arranged at the upper part of the transparent jacket, and a refrigerant flow regulating valve arranged at the heat exchange refrigerant inlet; by adjusting the refrigerant flow at the heat exchange refrigerant inlet, the temperature detected by the first temperature sensor is controlled at -40~-30℃, and the temperature detected by the second temperature sensor is controlled at -40~-30℃.

[0015] Preferably, the temperature in the intermediate buffer tank is controlled at -25-30°C; the temperature in the evaporation tank is controlled at -5-30°C, the material in the evaporation tank is gradually heated up and maintained for 30 minutes, and then the evaporation time is 2-3 hours.

[0016] Preferably, the first exhaust valve on the first exhaust pipe and the second exhaust valve on the second exhaust pipe remain normally open; the first exhaust gas discharge valve on the intermediate buffer tank and the second exhaust gas discharge valve on the evaporation tank remain normally open.

[0017] Preferably, the non-condensable gas in the photosynthetic reaction equipment is connected to the condenser through the non-condensable gas outlet pipe, the gas in the intermediate buffer tank is discharged into the condenser through the first exhaust pipe, and the gas in the evaporation tank is discharged into the condenser through the second exhaust pipe, and the temperature of the condenser is controlled at -50~-40°C; the hexafluoropropylene condensed by the condenser is discharged into the hexafluoropropylene recovery tank, and the non-condensable gas condensed by the condenser is discharged into the tail gas main pipe.

[0018] An industrial control system for perfluoropolyether acyl fluoride comprises photosynthetic reaction equipment, a metering pump, an intermediate buffer tank and an evaporation tank; the photosynthetic reaction equipment comprises a heat exchange column and a first temperature control unit, the first temperature control unit is used to adjust the refrigerant flow of the heat exchange column to achieve temperature control; a transparent jacket is arranged outside the heat exchange column, an ultraviolet lamp is arranged outside the transparent jacket, a spiral ring with openings at both ends is arranged inside the transparent jacket, the opening at the lower end of the spiral ring is connected to a material inlet pipe, a product outlet pipe and a non-condensable gas outlet pipe are arranged on the upper part of the transparent jacket, the material inlet pipe is connected to an oxygen inlet pipe and a hexafluoropropylene inlet pipe through a material control unit, and the material control unit is used to control the feed amount of oxygen and hexafluoropropylene; the product outlet pipe is connected to the intermediate buffer tank, and the intermediate buffer tank is connected to the evaporation tank through a third discharge pipe.

[0019] Preferably, the material control unit comprises an oxygen feed valve arranged on the oxygen inlet pipe and a hexafluoropropylene feed valve arranged on the hexafluoropropylene inlet pipe.

[0020] Preferably, the first temperature control unit includes a first temperature sensor arranged at the lower part of the transparent jacket, a second temperature sensor arranged at the upper part of the transparent jacket, and a refrigerant flow regulating valve arranged at the inlet of the heat exchange refrigerant.

[0021] Preferably, the second pressure sensor and the first pressure sensor are respectively provided at the upper and lower ends of the transparent jacket.

[0022] Preferably, the intermediate buffer tank and the evaporation tank are respectively provided with a first exhaust pipe and a second exhaust pipe, the first exhaust pipe, the second exhaust pipe and the non-condensable gas outlet pipe are all connected to the air inlet end of the condenser, the liquid outlet end of the condenser is connected to the hexafluoropropylene recovery tank through the liquid outlet pipe, and the gas outlet end of the condenser is connected to the tail gas main pipe.

[0023] Preferably, the intermediate buffer tank, the evaporation tank and the hexafluoropropylene recovery tank are respectively provided with a first tail gas emission pipe, a second tail gas emission pipe and a third tail gas emission pipe, and the first tail gas emission pipe, the second tail gas emission pipe and the third tail gas emission pipe are all connected to the tail gas main pipe.

[0024] Preferably, the spiral ring is provided with a plurality of openings; the plurality of openings are evenly arranged on the spiral ring.

[0025] The beneficial effects of this technical solution are as follows:

[0026] 1. The industrial control system for perfluoropolyether acyl fluoride provided by the present invention can realize the continuous photo-oxidative polymerization reaction control of ultraviolet light irradiation catalytic reaction of fluorinated olefins under low temperature conditions. Different from the traditional kettle-type intermittent reaction system, it can greatly shorten the reaction time and improve the reaction efficiency, and is suitable for large-scale industrial production.

[0027] 2. The industrial control system for perfluoropolyether fluoride provided by the present invention adopts an external ultraviolet light source to avoid direct contact between the light source and the reaction materials. Unlike the traditional kettle reactor, which often causes corrosion because the light source must be arranged in the kettle, affecting the normal reaction and even causing safety risks, it can greatly improve the stability and operability of the reaction system and is suitable for large-scale industrial production.

[0028] 3. The industrial control method for perfluoropolyether acyl fluoride provided by the present invention is a continuous flow reaction form, which is different from the traditional tank reactor. There is no material backmixing, and the reaction temperature and reaction residence time are stably controlled. Therefore, the product quality can be improved compared with the tank reaction form. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a process flow chart of the present invention;

[0030] Figure 2 It is a structural schematic diagram of the photosynthetic reaction equipment in the present invention.

[0031] Among them: 1. heat exchange column; 2. transparent jacket; 3. spiral ring; 4. material inlet pipe; 5. product outlet pipe; 6. non-condensable gas outlet pipe; 7. mixer; 8. oxygen inlet pipe; 9. hexafluoropropylene inlet pipe; 10. metering pump; 11. exhaust pipe; 12. first temperature sensor; 13. first pressure sensor; 14. second temperature sensor; 15. heat exchange refrigerant inlet; 16. heat exchange refrigerant outlet; 17. second pressure sensor; 100. photosynthetic reaction equipment; 200. intermediate buffer tank; 300. evaporation tank; 400. hexafluoropropylene recovery tank; 500. condenser; 600. tail gas main pipe; 610 , the first exhaust pipe; 620, the second exhaust pipe; 630, the third exhaust pipe; 710, the first exhaust pipe; 720, the second exhaust pipe; 810, the third exhaust pipe; 820, the fourth exhaust pipe; 910, the hexafluoropropylene feed valve; 920, the oxygen feed valve; 930, the first exhaust valve; 940, the second exhaust valve; 950, the first exhaust valve; 960, the second exhaust valve; 970, the first exhaust valve; 980, the second exhaust valve; 990, the third exhaust valve; 9100, the third exhaust valve; 9110, the fourth exhaust valve; 9120, the fifth exhaust valve. DETAILED DESCRIPTION

[0032] The present invention is further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.

[0033] like Figure 1 and Figure 2 As shown, an industrial control system for perfluoropolyether acyl fluoride includes a photosynthetic reaction device 100, a metering pump 10, an intermediate buffer tank 200, an evaporation tank 300, a hexafluoropropylene recovery tank 400 and a condenser 500;

[0034] The photosynthetic reaction equipment 100 includes a heat exchange column 1, a transparent jacket 2 is provided outside the heat exchange column 1, an ultraviolet lamp is provided outside the transparent jacket 2, a spiral ring 3 with openings at both ends is provided inside the transparent jacket 2, the opening at the lower end of the spiral ring 3 is connected to a material inlet pipe 4, a product outlet pipe 5 and a non-condensable gas outlet pipe 6 are provided at the upper part of the transparent jacket 2, and a drain pipe 11 is provided at the lower part of the transparent jacket 2;

[0035] The material inlet pipe 4 is connected to the oxygen inlet pipe 8 and the hexafluoropropylene inlet pipe 9 through a mixer 7, and the oxygen inlet pipe 8 and the hexafluoropropylene inlet pipe 9 are both provided with a metering pump 10;

[0036] The non-condensable gas outlet pipe 6 is connected to the condenser 500, the gas discharge port of the condenser 500 is connected to the tail gas main pipe 600, and the liquid discharge port of the condenser 500 is connected to the hexafluoropropylene recovery tank 400;

[0037] The product outlet pipe 5 and the discharge pipe 11 are connected to the intermediate buffer tank 200. The third discharge pipe 810 at the lower end of the intermediate buffer tank 200 is connected to the evaporation tank 300. The lower end of the evaporation tank 300 is provided with a fourth discharge pipe 820. The product outlet pipe 5 is provided with a second discharge valve 940, and the discharge pipe 11 is provided with a first discharge valve 930.

[0038] The first tail gas discharge pipe 610 at the upper end of the intermediate buffer tank 200, the second tail gas discharge pipe 620 at the upper end of the evaporation tank 300 and the third tail gas discharge pipe 630 at the upper end of the hexafluoropropylene recovery tank 400 are connected to the tail gas main pipe 600;

[0039] The first exhaust pipe 710 at the upper end of the intermediate buffer tank 200 and the second exhaust pipe 720 at the upper end of the evaporation tank 300 are connected to the condenser 500 .

[0040] The material inlet pipe 4 is connected to the oxygen inlet pipe 8 and the hexafluoropropylene inlet pipe 9 through the mixer 7 .

[0041] Wherein, both the oxygen inlet pipe 8 and the hexafluoropropylene inlet pipe 9 are provided with a metering pump 10 .

[0042] Wherein, a drain port is arranged at the lower end of the transparent jacket 2.

[0043] Wherein, a first temperature sensor 12 and a first pressure sensor 13 are arranged at the lower part of the transparent jacket 2 .

[0044] Wherein, a second temperature sensor 14 and a second pressure sensor 17 are arranged on the upper part of the transparent jacket 2 .

[0045] Wherein, the spiral ring 3 is provided with a plurality of openings.

[0046] Among them, multiple openings are evenly arranged on the screw ring 3.

[0047] The lower end of the heat exchange column 1 is provided with a heat exchange refrigerant inlet 15 , and the upper end of the heat exchange column 1 is provided with a heat exchange refrigerant outlet 16 .

[0048] Example 1

[0049] An industrial control method for perfluoropolyether acyl fluoride is adopted, comprising the following steps:

[0050] Step 1, hexafluoropropylene and oxygen flow into the mixer 7 through the hexafluoropropylene inlet pipe 9 and the oxygen inlet pipe 8 respectively, and the material control units on the hexafluoropropylene inlet pipe 9 and the oxygen inlet pipe 8 control the feed amounts of hexafluoropropylene and oxygen, so that the hexafluoropropylene and oxygen are fully mixed in the mixer 7 and atomized into a spray;

[0051] Step 2: The spray is continuously fed into the spiral ring 3 with openings at both ends in the photosynthetic reaction device 100, and the spray moves upward along the spiral ring 3. The spray reacts under the action of the ultraviolet lamp and the heat exchange column 1; the power of the ultraviolet lamp at the photosynthetic reaction device 100 and the first temperature control unit are controlled so that the spray reacts in the photosynthetic reaction device 100 to obtain a product liquid;

[0052] Step 3: The product liquid is discharged into the intermediate buffer tank 200 through the product outlet pipe 5, and finally discharged into the evaporation tank 300 through the third discharge pipe 810 for evaporation to obtain perfluoropolyether acyl fluoride.

[0053] The photosynthetic reaction device 100 has a height-to-diameter ratio of 10:1.

[0054] Wherein, the flow rate of the hexafluoropropylene inlet pipe 9 is 20Kg / h; the flow rate of the oxygen inlet pipe 8 is 0.5Kg / h.

[0055] Among them, the power of the ultraviolet lamp is controlled at 1500W, and the first temperature control unit includes a first temperature sensor 12 arranged at the lower part of the transparent jacket 2, a second temperature sensor 14 arranged at the upper part of the transparent jacket 2, and a refrigerant flow regulating valve arranged at the heat exchange refrigerant inlet 15; by adjusting the flow of the refrigerant at the heat exchange refrigerant inlet 15, the temperature detected by the first temperature sensor 12 is controlled at -30°C, and the temperature detected by the second temperature sensor 14 is controlled at -30°C.

[0056] The temperature in the intermediate buffer tank 200 is controlled at 30° C.; the temperature in the evaporation tank 300 is controlled at 30° C., the material in the evaporation tank 300 is gradually heated up and maintained for 30 minutes, and then the evaporation time is 2 hours.

[0057] The first exhaust valve 950 on the first exhaust pipe 710 and the second exhaust valve 960 on the second exhaust pipe 720 are kept open; the first exhaust gas discharge valve 970 on the intermediate buffer tank and the second exhaust gas discharge valve 980 on the evaporation tank 300 are kept open.

[0058] Among them, the non-condensable gas in the photosynthetic reaction equipment 100 is connected to the condenser 500 through the non-condensable gas outlet pipe 6, the gas in the intermediate buffer tank 200 is discharged into the condenser 500 through the first exhaust pipe 710, and the gas in the evaporation tank 300 is discharged into the condenser 500 through the second exhaust pipe 720. The temperature of the condenser 500 is controlled at -40°C; the hexafluoropropylene condensed by the condenser 500 is discharged into the hexafluoropropylene recovery tank 400, and the non-condensable gas condensed by the condenser 500 is discharged into the exhaust main pipe 600.

[0059] The yield of the obtained perfluoropolyether acyl fluoride is 6.5 Kg / h; the molecular weight is 820, the active oxygen content is 0.2%, and the conversion rate of hexafluoropropylene is 30.5%.

[0060] Example 2

[0061] The difference between this embodiment and embodiment 1 is that: the height-to-diameter ratio of the photosynthetic reaction device 100 is 15:1, the flow rate of the hexafluoropropylene inlet pipe 9 is 30Kg / h; the flow rate of the oxygen inlet pipe 8 is 3Kg / h; the power of the ultraviolet lamp is controlled at 2250W, the temperature detected by the first temperature sensor 12 is controlled at -35°C, the temperature detected by the second temperature sensor 14 is controlled at -35°C, the temperature detected by the temperature probe on the condenser 500 is controlled at -45°C, the temperature detected by the temperature probe on the intermediate buffer tank 200 is controlled at 12.5°C, and the temperature detected by the temperature probe on the evaporation tank 300 is controlled at 12.5°C.

[0062] The yield of the obtained perfluoropolyether acyl fluoride is 12.5 Kg / h; the molecular weight is 930, the active oxygen content is 0.23%, and the conversion rate of hexafluoropropylene is 40%.

[0063] Example 3

[0064] The difference between this embodiment and embodiment 1 is that the height-to-diameter ratio of the photosynthetic reaction device 100 is 20:1, the flow rate of the hexafluoropropylene inlet pipe 9 is 40Kg / h; the flow rate of the oxygen inlet pipe 8 is 5Kg / h; the power of the ultraviolet lamp is controlled at 3000W, the temperature detected by the first temperature sensor 12 is controlled at -40°C, the temperature detected by the second temperature sensor 14 is controlled at -40°C, the temperature detected by the temperature probe on the condenser 500 is controlled at -50°C, the temperature detected by the temperature probe on the intermediate buffer tank 200 is controlled at -5°C, and the temperature detected by the temperature probe on the evaporation tank 300 is controlled at -5°C.

[0065] The yield of the obtained perfluoropolyether acyl fluoride is 14.5 Kg / h; the molecular weight is 1050, the active oxygen content is 0.3%, and the conversion rate of hexafluoropropylene is 35%.

[0066] Comparative Example 1

[0067] The difference between this comparative example and Example 1 is that the flow rate of the hexafluoropropylene inlet pipe 9 is 15 Kg / h; the flow rate of the oxygen inlet pipe 8 is 0.5 Kg / h. The yield of the obtained perfluoropolyether acyl fluoride is 3.8 Kg / h; the molecular weight is 680, the active oxygen content is 0.28%, and the conversion rate of hexafluoropropylene is 25%.

[0068] Comparative Example 2

[0069] The difference between this comparative example and Example 3 is that the flow rate of the hexafluoropropylene inlet pipe 9 is 40 Kg / h; the flow rate of the oxygen inlet pipe 8 is 6 Kg / h. The yield of the obtained perfluoropolyether acyl fluoride is 11.5 Kg / h; the molecular weight is 850, the active oxygen content is 0.28%, and the conversion rate of hexafluoropropylene is 27%.

[0070] Comparative Example 3

[0071] The difference between this comparative example and Example 1 is that the power of the ultraviolet lamp is controlled at 1300W, the temperature detected by the first temperature sensor 12 is controlled at -30°C, and the temperature of the second temperature sensor 14 is controlled at -30°C. The yield of the obtained perfluoropolyether acyl fluoride is 4.2Kg / h, the molecular weight is 580, the active oxygen content is 0.3%, and the conversion rate of hexafluoropropylene is 20%.

[0072] Comparative Example 4

[0073] The difference between this comparative example and Example 3 is that the power of the ultraviolet lamp is controlled at 3200W, the temperature detected by the first temperature sensor 12 is controlled at -45°C, and the temperature detected by the second temperature sensor 14 is controlled at -45°C. The yield of the obtained perfluoropolyether acyl fluoride is 9.1Kg / h; the molecular weight is 1250, the active oxygen content is 0.2%, and the conversion rate of hexafluoropropylene is 22%.

[0074] Compared with Comparative Example 1, when the feed amounts of hexafluoropropylene and oxygen are too low, the active oxygen content increases and the conversion rate of hexafluoropropylene decreases in Example 1; when the oxygen feed amount is reduced in Example 3, the conversion rate of hexafluoropropylene is significantly reduced; when the power of the ultraviolet lamp is too low, the active oxygen content increases and the conversion rate of hexafluoropropylene decreases in Example 1; when the reaction temperature is too low, the conversion rate of hexafluoropropylene is significantly reduced in Example 4 compared with Comparative Example 3.

[0075] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent change made to the above embodiment based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. An industrial control method for perfluoropolyether acyl fluoride, characterized in that: The following steps are involved: Step 1: Hexafluoropropylene and oxygen flow into the mixer (7) through the hexafluoropropylene inlet pipe (9) and the oxygen inlet pipe (8) respectively; the material control units on the hexafluoropropylene inlet pipe (9) and the oxygen inlet pipe (8) control the feed amounts of hexafluoropropylene and oxygen, so that the hexafluoropropylene and oxygen are fully mixed in the mixer (7) and atomized into a spray; the flow rate on the hexafluoropropylene inlet pipe (9) is 20-40 kg / h; the flow rate on the oxygen inlet pipe (8) is 0.5-5 kg / h; Step 2: The spray is continuously fed into a spiral ring (3) with openings at both ends in the photosynthetic reaction device (100), the spray moves upward along the spiral ring (3), and the spray reacts under the action of the ultraviolet lamp and the heat exchange column (1); the power of the ultraviolet lamp and the first temperature control unit at the photosynthetic reaction device (100) are controlled so that the spray reacts in the photosynthetic reaction device (100) to obtain a product liquid; Step 3: The product liquid is discharged into the intermediate buffer tank (200) through the product outlet pipe (5), and finally discharged into the evaporation tank (300) through the third discharge pipe (810) for evaporation to obtain perfluoropolyether acyl fluoride.

2. The industrial control method for perfluoropolyether acyl fluoride according to claim 1, characterized in that: The photosynthetic reaction device (100) has a height-to-diameter ratio of 10-20:

1.

3. The industrial control method for perfluoropolyether acyl fluoride according to claim 2, characterized in that: The power of the ultraviolet lamp is controlled at 1500-3000W, and the first temperature control unit comprises a first temperature sensor (12) arranged at the bottom of the transparent jacket (2), a second temperature sensor (14) arranged at the top of the transparent jacket (2), and a refrigerant flow regulating valve arranged at the heat exchange refrigerant inlet (15); by adjusting the refrigerant flow at the heat exchange refrigerant inlet (15), the temperature detected by the first temperature sensor (12) is controlled at -40--30°C, and the temperature detected by the second temperature sensor (14) is controlled at -40--30°C; the temperature in the intermediate buffer tank (200) is controlled at -25-30°C; the temperature in the evaporation tank (300) is controlled at -5-30°C, and the material in the evaporation tank (300) is gradually heated up and maintained for 30 minutes, and then the evaporation time is 2-3 hours.

4. The industrial control method for perfluoropolyether acyl fluoride according to claim 3, characterized in that: The first exhaust valve (950) on the first exhaust pipe (710) and the second exhaust valve (960) on the second exhaust pipe (720) remain normally open; the first exhaust gas discharge valve (970) on the intermediate buffer tank (200) and the second exhaust gas discharge valve (980) on the evaporation tank (300) remain normally open.

5. The industrial control method for perfluoropolyether acyl fluoride according to claim 4, characterized in that: The non-condensable gas in the photosynthetic reaction device (100) is connected to the condenser (500) via the non-condensable gas outlet pipe (6), the gas in the intermediate buffer tank (200) is discharged into the condenser (500) via the first exhaust pipe (710), and the gas in the evaporation tank (300) is discharged into the condenser (500) via the second exhaust pipe (720), and the temperature of the condenser (500) is controlled at -50 to -40°C; The hexafluoropropylene condensed by the condenser (500) is discharged into the hexafluoropropylene recovery tank (400), and the non-condensable gas condensed by the condenser (500) is discharged into the tail gas main pipe (600).

6. The industrial control system used in the industrial control method for perfluoropolyether acyl fluoride according to any one of claims 1 to 5, characterized in that: The invention comprises a photosynthetic reaction device (100), a metering pump (10), an intermediate buffer tank (200) and an evaporation tank (300); the photosynthetic reaction device (100) comprises a heat exchange column (1) and a first temperature control unit, the first temperature control unit being used to adjust the flow rate of a refrigerant of the heat exchange column (1) so as to achieve temperature control; a transparent jacket (2) is arranged outside the heat exchange column (1), an ultraviolet lamp is arranged outside the transparent jacket (2), a spiral ring (3) with two ends open is arranged inside the transparent jacket (2), and the spiral ring (3) The opening at the lower end is connected to the material inlet pipe (4); the upper part of the transparent jacket (2) is provided with a product outlet pipe (5) and a non-condensable gas outlet pipe (6); the material inlet pipe (4) is connected to the oxygen inlet pipe (8) and the hexafluoropropylene inlet pipe (9) through a material control unit; the material control unit is used to control the feed amount of oxygen and hexafluoropropylene; the product outlet pipe (5) is connected to the intermediate buffer tank (200), and the intermediate buffer tank (200) is connected to the evaporation tank (300) through a third discharge pipe (810).

7. An industrial control system for perfluoropolyether acyl fluoride according to claim 6, characterized in that: The material control unit comprises an oxygen feed valve (920) arranged on an oxygen feed pipe (8) and a hexafluoropropylene feed valve (910) arranged on a hexafluoropropylene feed pipe (9).

8. An industrial control system for perfluoropolyether acyl fluoride according to claim 7, characterized in that: The first temperature control unit comprises a first temperature sensor (12) arranged at the bottom of the transparent jacket (2), a second temperature sensor (14) arranged at the top of the transparent jacket (2), and a refrigerant flow regulating valve arranged at the heat exchange refrigerant inlet (15).

9. An industrial control system for perfluoropolyether acyl fluoride according to claim 8, characterized in that: The transparent jacket (2) is provided with a second pressure sensor (17) and a first pressure sensor (13) at the upper and lower ends, respectively.

10. An industrial control system for perfluoropolyether acyl fluoride according to claim 9, characterized in that: The intermediate buffer tank (200) and the evaporation tank (300) are respectively provided with a first exhaust pipe (710) and a second exhaust pipe (720); the first exhaust pipe (710), the second exhaust pipe (720) and the non-condensable gas outlet pipe (6) are all connected to the gas inlet end of the condenser (500); the liquid outlet end of the condenser (500) is connected to the hexafluoropropylene recovery tank (400) via the liquid outlet pipe; and the gas outlet end of the condenser (500) is connected to the tail gas main pipe (600).

11. An industrial control system for perfluoropolyether acyl fluoride according to claim 10, characterized in that: The intermediate buffer tank (200), the evaporation tank (300) and the hexafluoropropylene recovery tank (400) are respectively provided with a first tail gas emission pipe (610), a second tail gas emission pipe (620) and a third tail gas emission pipe (630); the first tail gas emission pipe (610), the second tail gas emission pipe (620) and the third tail gas emission pipe (630) are all connected to the tail gas main pipe (600).

12. An industrial control system for perfluoropolyether acyl fluoride according to claim 11, characterized in that: The spiral ring (3) is provided with a plurality of openings; the plurality of openings are evenly arranged on the spiral ring (3).

Citation Information

Patent Citations

  • Process system and method for synthesizing perfluoropolyether with medium and low molecular weights

    CN116637574A

  • Industrial control method and system for efficiently synthesizing perfluoropolyether acyl fluoride

    CN117680071A

  • Method for preparing perfluoropolyether acyl fluoride through continuous cross-flow photooxidation reaction

    CN118546351A

  • Novel multi-flux continuous photoreactor and system thereof

    CN210357115U