Apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane

CN224748564UActive Publication Date: 2026-09-15NEWERA CHEM SHANDONG CO LTD +1
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Patent Information

Application Number
CN202522650386.7
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-12-15
Publication Date
2026-09-15
Estimated Expiration
2035-12-15

AI Technical Summary

Technical Problem

本实用新型采用集成设计,从本质上解决了传统D3F生产高排放、高能耗、间歇式的问题,实现了向绿色、连续、高效生产的升级

Benefits of technology

1、实现连续化生产,提升效率与质量:通过多釜/塔并联、切换及物料连续输送的设计,突破了传统间歇工艺的瓶颈,显著提高了生产效率,并保证了产品质量的稳定性和一致性。

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the device of continuous production trifluoropropyl methyl cyclotrisiloxane, and the device includes pre -splitting dehydration system, continuous cracking rectification system, continuous product rectification system, front fraction recovery rectification system, impurity rectification system and tail gas treatment system of sequential intercommunication, the utility model discloses adopts the parallel connection design of multiple reaction / rectification unit and realizes continuous production, constructs the whole process material recovery network of four -stage rectification and tail gas deep condensation combination, greatly promotes product yield, designs full -seal negative pressure tail gas collection system, ensures vacuum stability and will VOCs unorganized emission to the minimum, the utility model solves the problem of traditional process intermittent, low efficiency, high emission, is applicable to the green, efficient, large -scale industrial production of D3F.
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Description

Technical Field

[0001] This utility model relates to the field of chemical production equipment technology, and more specifically, to an apparatus for the continuous and efficient production of trifluoropropylmethylcyclotrisiloxane. Background Technology

[0002] Trifluoropropylmethylcyclotrisiloxane (D3F) is an indispensable key monomer in the synthesis of organofluorosilicone materials. Introducing it into the polymer backbone yields high-end materials possessing the superior properties of both organosilicon and organofluorine compounds, widely used in specialty rubbers, weather-resistant coatings, high-efficiency lubricants, and electronic packaging. Fluorosilicone rubber synthesized from D3F exhibits excellent oil, solvent, and chemical resistance, as well as good cold and heat resistance, earning it the reputation as one of the best-performing synthetic rubbers. It is crucial in seals, oil pipes, and other components used in extreme environments such as aerospace and automotive industries.

[0003] D3F is mainly obtained by hydrolyzing trifluoropropylmethyldichlorosilane and then reacting it with a base in a cyclization reaction. The main reaction equations are as follows: .

[0004] For example, CN119504841A and CN117820360A both disclose the preparation process of D3F. However, neither of these methods mentions how to achieve industrial scale-up. At the same time, the exhaust gas and high-boiling residue generated during the production process are hazardous wastes, and their compliant disposal is also a problem faced in the industrial production process.

[0005] In addition, CN204569787U discloses a reactor system for preparing trifluoropropylmethylcyclotrisiloxane, but the reactor system adopts intermittent operation, which has the disadvantages of low automation, high labor intensity and poor batch-to-batch quality stability. Summary of the Invention

[0006] In view of the aforementioned state of the prior art, the purpose of this invention is to provide an apparatus suitable for the continuous industrial production of trifluoropropylmethylcyclotrisiloxane (D3F). This apparatus achieves high-purity and high-yield production of D3F products through a multi-stage, multi-sequence distillation separation process. By constructing a waste gas collection and staged condensation recovery system, valuable components such as D3F in the process waste gas are recovered to the greatest extent, significantly reducing the load and operating costs of subsequent waste gas treatment equipment and improving the overall yield of D3F products. This invention adopts an integrated design, fundamentally solving the problems of high emissions, high energy consumption, and intermittent operation in traditional D3F production, and achieving an upgrade to green, continuous, and efficient production.

[0007] The technical solution of this utility model can be summarized as follows: An apparatus for the continuous production of trifluoropropylmethylcyclotrisiloxane, comprising a pre-cracking and dehydration system, a continuous cracking and distillation system, a continuous product distillation system, a fore-fraction recovery and distillation system, an impurity distillation system, and a tail gas treatment system connected in sequence. The pre-pyrolysis dehydration system includes a pre-pyrolysis vessel equipped with a vacuum dehydration device, and the top of the pre-pyrolysis vessel is connected to a buffer tank through a pre-pyrolysis condenser. The continuous cracking distillation system includes a first cracking vessel, the top of which is connected to a first cracking distillation column, the top of which is connected to a buffer tank via a first cracking distillation column condenser, and the bottom of which is connected to a desiccation vessel, which is a vacuum distillation device, with a desiccation vessel condenser connected to its top. A pre-cracking vessel is connected to the first cracking vessel via a pre-cracking feed pump. The continuous product distillation system includes a first product distillation column, the top of which is connected to a buffer tank via a first product distillation column condenser, the upper part of which is connected to a first fore-distillate tank, a first high-distillate tank, and a product storage tank, the first high-distillate tank being connected to the lower part of the first product distillation column, and the upper part of the first cracking distillation column being connected to the middle part of the first product distillation column via a crude product tank and a distillation feed pump; The fore-distillate recovery and rectification system includes a fore-distillate distillation kettle, the top of which is connected to a fore-distillate distillation column, the top of which is connected to a buffer tank via a fore-distillate condenser, the upper part of which is connected to a first light component tank, an impurity receiving tank, and a product storage tank, respectively, and the bottom of the forced-drying kettle condenser and the bottom of the first fore-distillate tank are respectively connected to the fore-distillate distillation kettle. The impurity distillation system includes an impurity distillation kettle, an impurity distillation column connected to the top of the impurity distillation kettle, a buffer tank connected to the impurity distillation column via an impurity condenser, a high-boiling component tank and a light component tank connected to the upper part of the impurity distillation column, and an impurity distillation kettle connected to the bottom of the high-boiling component tank and the bottom of the impurity receiving tank. The exhaust gas treatment system includes an exhaust gas receiving tank, at least two exhaust gas condensers are installed on the top of the exhaust gas receiving tank, at least one exhaust gas condenser is connected to a buffer tank via a vacuum pump, and at least one exhaust gas condenser is connected to an exhaust gas treatment device via an induced draft fan; the bottom of the exhaust gas receiving tank is connected to a crude product tank via a light component pump.

[0008] According to this utility model, preferably, the pre-pyrolysis dehydration system further includes a metering tank, which is connected to the pre-pyrolysis vessel via a pre-pyrolysis feed pump; Preferably, the pre-pyrolysis dehydration system further includes a pre-pyrolysis intermediate tank disposed between the pre-pyrolysis vessel and the first pyrolysis vessel, and the pre-pyrolysis vessel is connected to the pre-pyrolysis intermediate tank via a pre-pyrolysis feed pump.

[0009] According to the present invention, preferably, the continuous cracking distillation system further includes a crude product receiving tank disposed between the first cracking distillation column and the crude product tank, and the crude product receiving tank is connected to the crude product tank through a crude product feed pump; Preferably, the first cracking vessel, the first cracking distillation column, and the first cracking distillation column condenser are combined to form a cracking distillation unit, and the continuous cracking distillation system includes at least two cracking distillation units connected in parallel.

[0010] According to this utility model, preferably, the continuous product distillation system further includes a first product receiving tank located between the first product distillation column and the product storage tank; Preferably, the first product distillation column, the first product distillation column condenser, the first pre-distillate tank, the first high-distillate tank, and the first product receiving tank are combined to form a product distillation unit, and the continuous product distillation system includes at least two product distillation units connected in parallel. Preferably, the number of product storage tanks is at least two, connected in parallel; Preferably, a product pump is connected to the bottom of the product storage tank.

[0011] According to this utility model, preferably, the fore-fraction recovery distillation system further includes a product receiving tank located between the fore-fraction distillation column and the product storage tank.

[0012] The beneficial effects of this utility model are as follows: 1. Achieve continuous production and improve efficiency and quality: Through the design of parallel connection, switching and continuous material conveying of multiple reactors / towers, the bottleneck of traditional intermittent processes is broken through, significantly improving production efficiency and ensuring the stability and consistency of product quality.

[0013] 2. High resource recovery rate and significant economic benefits: The entire process material recovery network adopts a four-stage recovery system, including product distillation, fore-distillation, impurity distillation, and forced-drying kettle recovery, plus tail gas condensation. This achieves closed-loop reuse and recovery from the main product to the middle fraction, improving the overall yield of D3F and reducing raw material consumption.

[0014] 3. Energy saving and emission reduction, excellent environmental performance: The integrated exhaust gas treatment system and deep condensation reduce the emission of VOCs from the source, and significantly reduce the load and operating cost of the exhaust gas treatment device. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the main structure of this utility model.

[0016] The components are as follows: 1. Metering tank; 2. Pre-cracking feed pump; 3. Pre-cracking vessel; 4. Pre-cracking feed pump; 5. Pre-cracking condenser; 6. Pre-cracking intermediate tank; 7. First cracking vessel; 8. First cracking distillation column; 9. First cracking distillation column condenser; 10. Second cracking vessel; 11. Second cracking distillation column; 12. Second cracking distillation column condenser; 13. Crude product receiving tank; 14. Crude product feed pump; 15. Crude product tank; 16. Distillation feed pump; 17. First product distillation column; 18. First product distillation column condenser; 19. First fore-fraction tank; 20. First high-fraction tank; 21. First product receiving tank; 22. Second product distillation column; 23. Second product distillation column. 24. Second fore-distillation tank, 25. Second high-distillation tank, 26. Second product receiving tank, 27. Product storage tank, 28. Product pump, 29. Fore-distillation kettle, 30. Fore-distillation column, 31. Fore-distillation condenser, 32. First light component tank, 33. Second light component tank, 34. Impurity receiving tank, 35. Product receiving tank, 36. Impurity distillation kettle, 37. Impurity distillation column, 38. Impurity condenser, 39. High-boiling component tank, 40. Light component tank, 41. Forced-drying kettle, 42. Forced-drying kettle condenser, 43. Buffer tank, 44. Vacuum pump, 45. Tail gas receiving tank, 46. Tail gas condenser, 47. Light component pump, 48. Exhaust fan. Detailed Implementation

[0017] The D3F production method applicable to this invention mainly involves the hydrolysis of trifluoropropylmethyldichlorosilane followed by a cyclization reaction with an alkali. The main reaction equations are as follows:

[0018] The specific equipment used in the apparatus for the continuous production of trifluoropropylmethylcyclotrisiloxane of this invention are all conventional chemical equipment. For example, the tanks used include metering tank 1, pre-cracking intermediate tank 6, crude product receiving tank 13, crude product tank 15, first pre-distillate tank 19, first high-distillate tank 20, first product receiving tank 21, second pre-distillate tank 24, second high-distillate tank 25, second product receiving tank 26, product storage tank 27, first light component tank 32, second light component tank 33, impurity receiving tank 34, product receiving tank 35, high-boiling component tank 39, light component tank 40, buffer tank 43, and tail gas receiving tank 45, all of which are conventional corrosion-resistant pressure vessels or atmospheric pressure vessels in the chemical industry.

[0019] The reactor equipment used includes a pre-cracking reactor 3, a first cracking reactor 7, a second cracking reactor 10, a pre-fraction distillation reactor 29, an impurity distillation reactor 36, and a desiccation reactor 41. All are conventional pressure-resistant reactors, equipped with heating devices to meet the temperature requirements of different reactions. Far-infrared heaters can be used for these heating devices. The reactor equipment can also be connected to a vacuum system. For example, the pre-cracking reactor 3, first cracking reactor 7, second cracking reactor 10, pre-fraction distillation reactor 29, impurity distillation reactor 36, and desiccation reactor 41 can be connected to a vacuum system to achieve negative pressure heating, facilitating reactions under different conditions. In scenarios requiring stirring, stirring devices can be installed inside the reactor equipment. For example, the pre-cracking reactor 3, first cracking reactor 7, second cracking reactor 10, pre-fraction distillation reactor 29, impurity distillation reactor 36, and desiccation reactor 41 are equipped with stirring blades, which are connected to an external stirring motor via a stirring shaft. A residual liquid discharge valve is located at the bottom of the reactor to periodically discharge residual liquid.

[0020] The distillation equipment used includes a first cracking distillation column 8, a second cracking distillation column 11, a first product distillation column 17, a second product distillation column 22, a fore-fraction distillation column 30, and an impurity distillation column 37, all of which are conventional distillation equipment. The bottom of each distillation column is a reboiler equipped with a heating device to heat the material to be heated. The column body is equipped with trays and packing. A side stream is collected from the upper part of the distillation column. The location of the side stream can be connected to a fraction analysis or temperature control system. Each fraction enters a corresponding tank according to online analysis or temperature control. For example, the upper part of the first product distillation column 17 is connected to a fraction analysis or temperature control system. The fore-fraction (low-boiling fraction) is fed into the first fore-fraction receiving tank 19, product D3F is fed into the first product receiving tank 21, and the intermediate high-boiling fraction is fed into the first high-fraction tank 20 and then refluxed back into the first product distillation column 17 for reuse. The upper part of the pre-fraction distillation column 30 is connected to a fraction analysis or temperature control system, which directs components of different purity ranges into different tanks. For example, components with a purity of 90%-95% are directed into light component tanks 32 and 33 and then returned to the pre-fraction distillation kettle 29 for reuse. Components with a purity of 95%-99% are directed into impurity receiving tank 34 and then into impurity distillation kettle 36 for further distillation separation. D3F product is directed into product receiving tank 35. The upper part of the impurity distillation column 37 is connected to a fraction analysis or temperature control system, which directs components with different boiling points into different tanks. For example, high-boiling fractions are directed into high-boiling fraction tank 39 and then returned to impurity distillation kettle 36 for reuse, while low-boiling fractions are directed into light component tank 40 for solid waste disposal.

[0021] The condensation equipment used includes a pre-cracking condenser 5, a first cracking distillation column condenser 9, a second cracking distillation column condenser 12, a first product distillation column condenser 18, a second product distillation column condenser 23, a fore-fraction condenser 31, an impurity condenser 38, a forced-drying kettle condenser 42, and a tail gas condenser 46, all of which are conventional heat exchange equipment, such as shell and tube heat exchangers. In the first cracking distillation column 8, the second cracking distillation column 11, the first product distillation column 17, the second product distillation column 22, the fore-fraction distillation column 30, and the impurity distillation column 37, the components are condensed and refluxed through the condensers, different fraction side streams are collected, and the uncondensed components enter the buffer tank 43 for further processing.

[0022] The pumps used include a pre-cracking feed pump 2, a pre-cracking feed pump 4, a distillation feed pump 16, a product pump 28, a vacuum pump 44, and a light component pump 47, all of which are conventional transfer pumps or vacuum pumps. For example, vacuum pump 44 can be a corrosion-resistant dry screw vacuum pump. This type of pump does not require a working fluid and can stably contact and transport complex process gases containing D3F, water vapor, and trace amounts of acidic components for a long time. This avoids the problems of vacuum attenuation and frequent maintenance caused by oil contamination and emulsification in traditional oil pumps, making it particularly suitable for the harsh operating conditions of this process. Pre-cracking feed pump 2, pre-cracking feed pump 4, distillation feed pump 16, product pump 28, and light component pump 47 all use corrosion-resistant pump materials.

[0023] This invention can be connected to a centralized control and online monitoring system, such as an existing DCS system, to achieve centralized control and online monitoring. Important parameters such as temperature, pressure, and vacuum can be automatically adjusted and interlocked with alarms, reducing manual operation and improving the safety and controllability of the production process. This invention uses parallel pyrolysis reactors and distillation columns, and can be equipped with automatic switching valve groups, enabling a continuous production mode where one column is running online while the other is on standby or under maintenance, thus ensuring the long-term continuous and stable operation of the entire unit.

[0024] The embodiments of the present invention will be described in detail below with reference to the accompanying drawings, but the implementation of the present invention is not limited thereto.

[0025] Example 1 like Figure 1 As shown, an apparatus for the continuous production of trifluoropropylmethylcyclotrisiloxane includes a pre-cracking and dehydration system, a continuous cracking and distillation system, a continuous product distillation system, a fore-fraction recovery and distillation system, an impurity distillation system, and a tail gas treatment system connected in sequence. The pre-pyrolysis dehydration system includes a pre-pyrolysis vessel 3 equipped with a vacuum dehydration device, and the top of the pre-pyrolysis vessel 3 is connected to a buffer tank 43 through a pre-pyrolysis condenser 5. The continuous cracking distillation system includes a first cracking vessel 7, the top of which is connected to a first cracking distillation column 8, the top of which is connected to a buffer tank 43 via a first cracking distillation column condenser 9, and the bottom of which is connected to a desiccation vessel 41, which is a vacuum distillation device, with a desiccation vessel condenser 42 connected to the top of the desiccation vessel 41; a pre-cracking vessel 3 is connected to the first cracking vessel 7 via a pre-cracking feed pump 4. The continuous product distillation system includes a first product distillation column 17. The top of the first product distillation column 17 is connected to a buffer tank 43 via a first product distillation column condenser 18. The upper part of the first product distillation column 17 is connected to a first fore-distillate tank 19, a first high-distillate tank 20, and a product storage tank 27. The first high-distillate tank 20 is connected to the lower part of the first product distillation column 17. The upper part of the first cracking distillation column 8 is connected to the middle part of the first product distillation column 17 via a crude product tank 15 and a distillation feed pump 16. The fore-distillate recovery and rectification system includes a fore-distillate distillation kettle 29, the top of which is connected to a fore-distillate distillation column 30. The top of the fore-distillate distillation column 30 is connected to a buffer tank 43 via a fore-distillate condenser 31. The upper part of the fore-distillate condenser 31 is connected to a first light component tank 32, an impurity receiving tank 34, and a product storage tank 27, respectively. The bottom of the forced-drying kettle condenser 42 and the bottom of the first fore-distillate tank 19 are respectively connected to the fore-distillate distillation kettle 29. The impurity distillation system includes an impurity distillation kettle 36, an impurity distillation column 37 connected to the top of the impurity distillation kettle 36, a buffer tank 43 connected to the impurity distillation column 37 via an impurity condenser 38, a high-boiling component tank 39 and a light component tank 40 connected to the upper part of the impurity distillation column 37 respectively, and the bottom of the high-boiling component tank 39 and the bottom of the impurity receiving tank 34 connected to the impurity distillation kettle 36 respectively. The exhaust gas treatment system includes an exhaust gas receiving tank 45, at least two exhaust gas condensers 46 are provided on the top of the exhaust gas receiving tank 45, at least one exhaust gas condenser 46 is connected to a buffer tank 43 through a vacuum pump 44, and at least one exhaust gas condenser 46 is connected to an exhaust gas treatment device through an induced draft fan 48; the bottom of the exhaust gas receiving tank 45 is connected to a crude product tank 15 through a light component pump 47.

[0026] Example 2 As described in Example 1, the difference is: The pre-pyrolysis dehydration system also includes a metering tank 1, which is connected to the pre-pyrolysis vessel 3 via a pre-pyrolysis feed pump 2. The pre-pyrolysis dehydration system also includes a pre-pyrolysis intermediate tank 6 disposed between the pre-pyrolysis vessel 3 and the first pyrolysis vessel 7. The pre-pyrolysis vessel 3 is connected to the pre-pyrolysis intermediate tank 6 via a pre-pyrolysis feed pump 4.

[0027] Example 3 As described in Example 2, the difference is: The continuous cracking distillation system also includes a crude product receiving tank 13 disposed between the first cracking distillation column 8 and the crude product tank 15, and the crude product receiving tank 13 is connected to the crude product tank 15 through a crude product feed pump 14. The first cracking vessel 7, the first cracking distillation column 8, and the first cracking distillation column condenser 9 are combined to form a cracking distillation unit. The continuous cracking distillation system includes two sets of cracking distillation units connected in parallel. The second cracking vessel 10, the second cracking distillation column 11, and the second cracking distillation column condenser 12 are combined to form a second set of cracking distillation units.

[0028] Example 4 As described in Example 3, the difference is: The continuous product distillation system also includes a first product receiving tank 21 located between the first product distillation column 17 and the product storage tank 27; The first product distillation column 17, the first product distillation column condenser 18, the first pre-distillate tank 19, the first high-distillate tank 20, and the first product receiving tank 21 together constitute a product distillation unit. The continuous product distillation system includes two sets of product distillation units connected in parallel. The second product distillation column 22, the second product distillation column condenser 23, the second pre-distillate tank 24, the second high-distillate tank 25, and the second product receiving tank 26 together constitute a second set of product distillation units.

[0029] Example 5 As described in Example 4, the difference is: The product storage tank 27 consists of two tanks connected in parallel, and the bottom of the product storage tank 27 is connected to a product pump 28. The fore-fraction recovery distillation system also includes a product receiving tank 35 located between the fore-fraction distillation column 30 and the product storage tank 27.

[0030] A preferred operating process of this utility model is as follows: 1. Pre-pyrolysis Dehydration System: The hydrolysate of trifluoropropylmethyldichlorosilane is transported from the upstream workshop to the hydrolysate metering tank 1. It is pumped into the pre-pyrolysis reactor 3, which includes a vacuum dehydration device and far-infrared heating, via the pre-pyrolysis feed pump 2, and dehydrated under vacuum at approximately 70°C and -0.098 MPa for 2 hours. After dehydration, the pressure is restored to normal, and sodium hydroxide solution is added and reacted at 70-80°C for 2 hours. Vacuuming is then performed again, and the temperature is raised to 120-150°C for deep dehydration. After dehydration, the material is temporarily stored in the pre-pyrolysis intermediate tank 6 via the pre-pyrolysis feed pump 4. Water vapor generated during the dehydration process is condensed and collected for treatment by the pre-pyrolysis condenser 5.

[0031] 2. Continuous Cracking and Distillation System: The material in the pre-cracking intermediate tank 6 flows into the parallel cracking reactors 7 and 10. Cracking reactors 7 and 10 are equipped with stirring devices, far-infrared heating devices, and are connected to a vacuum system. The integrated vacuum system maintains the temperature within cracking reactors 7 and 10 at 175-205℃ and the vacuum degree at -0.098MPa. The material is condensed by the corresponding cracking distillation column condensers 9 and 12. A portion of the condensate is continuously collected as product and sent to the crude product receiving tank 13. The crude product is then transported to the crude product storage tank 16 by the crude product feed pump 14. High-boiling-point substances in cracking reactors 7 and 10 are periodically discharged into the desiccant tank 41 for vacuum distillation to further recover residual D3F. The residue is then disposed of as hazardous waste.

[0032] 3. Continuous Product Distillation System: The material in crude product storage tank 16 is distilled through parallel product distillation columns 17 and 22. The top fraction is condensed by distillation column condensers 18 and 23. Based on temperature or online analysis control, the fore-distillate (low-boiling fraction) is sent to fore-distillate receiving tanks 19 and 24, product D3F is sent to product receiving tanks 21 and 26, and the intermediate high-boiling fraction is sent to high-distillate tanks 20 and 25 and then returned to product distillation columns 17 and 22 for reuse. After passing analysis, the product in product receiving tanks 21 and 26 is sent to product storage tank 27.

[0033] 4. Fore-fraction recovery and distillation system, and impurity distillation system: The material in the fore-fraction receiving tanks 19 and 24 is conveyed to the fore-fraction distillation kettle 29 and then enters the fore-fraction distillation column 30 for re-distillation, separating components of different purities. Low-purity components (e.g., 90-95%) enter the impurity receiving tank 34 and are sent to the impurity distillation kettle 36; medium- and high-purity components enter the light component tanks 32 and 33 and are returned to the fore-fraction distillation kettle 29 for reuse; D3F that meets product standards is sent to the product storage tank 27. Low-purity material from the fore-fraction recovery and distillation system is further separated in the impurity distillation kettle 36 and the impurity distillation column 37. The <60% extremely low boiling fraction is disposed of as waste, the 60-95% component enters the light component tank 40, and the >95% component is returned to the fore-fraction distillation system for reuse.

[0034] 5. Exhaust Gas Treatment System: All process waste gases described above are drawn into the exhaust gas treatment system in a closed loop. The gas first enters the buffer tank 43 for buffering, and then is transported by the corrosion-resistant dry screw vacuum pump 44 to the exhaust gas condenser 46. Here, most of the D3F, water, and organosilicon intermediates in the waste gas are condensed and flow into the exhaust gas receiving tank 45, where they are pumped back to the crude product tank 16 for recovery by the light component pump 47, greatly improving the product yield. After condensation and recovery, the volume of non-condensable exhaust gas is greatly reduced, and finally, it is sent to the centralized waste gas treatment unit in the plant area for final disposal by the induced draft fan 48.

[0035] This invention, through the coordinated operation of the above systems, realizes the entire process from feeding, pyrolysis, distillation to waste gas treatment. The entire process is continuous and closed, with significant advantages such as high product yield, stable quality, low energy and material consumption, environmental compliance, and reliable operation.

Claims

1. An apparatus for the continuous production of trifluoropropylmethylcyclotrisiloxane, characterized in that, The device includes a pre-cracking and dehydration system, a continuous cracking and distillation system, a continuous product distillation system, a fore-fraction recovery and distillation system, an impurity distillation system, and a tail gas treatment system connected in sequence. The pre-pyrolysis dehydration system includes a pre-pyrolysis vessel (3) equipped with a vacuum dehydration device, and the top of the pre-pyrolysis vessel (3) is connected to a buffer tank (43) through a pre-pyrolysis condenser (5). The continuous cracking distillation system includes a first cracking vessel (7), the top of which is connected to a first cracking distillation column (8), the top of which is connected to a buffer tank (43) via a first cracking distillation column condenser (9), and the bottom of which is connected to a desiccant (41), which is a vacuum distillation device, and the top of which is connected to a desiccant condenser (42); a pre-cracking vessel (3) is connected to the first cracking vessel (7) via a pre-cracking feed pump (4); The continuous product distillation system includes a first product distillation column (17), the top of the first product distillation column (17) is connected to a buffer tank (43) through a first product distillation column condenser (18), the upper part of the first product distillation column (17) is connected to a first pre-distillate tank (19), a first high-distillate tank (20) and a product storage tank (27), the first high-distillate tank (20) is connected to the lower part of the first product distillation column (17), and the upper part of the first cracking distillation column (8) is connected to the middle part of the first product distillation column (17) through a crude product tank (15) and a distillation feed pump (16); The fore-distillation recovery system includes a fore-distillation kettle (29), the top of which is connected to a fore-distillation column (30), the top of which is connected to a buffer tank (43) via a fore-distillation condenser (31), the upper part of which is connected to a first light component tank (32), an impurity receiving tank (34) and a product storage tank (27), and the bottom of the forced-drying kettle condenser (42) and the bottom of the first fore-distillation tank (19) are respectively connected to the fore-distillation kettle (29); The impurity distillation system includes an impurity distillation kettle (36), the top of which is connected to an impurity distillation column (37), the impurity distillation column (37) is connected to a buffer tank (43) through an impurity condenser (38), the upper part of the impurity distillation column (37) is connected to a high-boiling component tank (39) and a light component tank (40), and the bottom of the high-boiling component tank (39) and the bottom of the impurity receiving tank (34) are respectively connected to the impurity distillation kettle (36). The exhaust gas treatment system includes an exhaust gas receiving tank (45), at least two exhaust gas condensers (46) are provided on the top of the exhaust gas receiving tank (45), at least one exhaust gas condenser (46) is connected to a buffer tank (43) through a vacuum pump (44), and at least one exhaust gas condenser (46) is connected to an exhaust gas treatment device through an induced draft fan (48); the bottom of the exhaust gas receiving tank (45) is connected to a crude product tank (15) through a light component pump (47).

2. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 1, characterized in that, The pre-pyrolysis dehydration system also includes a metering tank (1), which is connected to the pre-pyrolysis vessel (3) via a pre-pyrolysis feed pump (2).

3. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 2, characterized in that, The pre-pyrolysis dehydration system also includes a pre-pyrolysis intermediate tank (6) located between the pre-pyrolysis vessel (3) and the first pyrolysis vessel (7). The pre-pyrolysis vessel (3) is connected to the pre-pyrolysis intermediate tank (6) via a pre-pyrolysis feed pump (4).

4. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 3, characterized in that, The continuous cracking distillation system also includes a crude product receiving tank (13) located between the first cracking distillation column (8) and the crude product tank (15), and the crude product receiving tank (13) is connected to the crude product tank (15) via a crude product feed pump (14).

5. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to any one of claims 1-4, characterized in that, The first cracking vessel (7), the first cracking distillation column (8) and the first cracking distillation column condenser (9) are combined to form a cracking distillation unit. The continuous cracking distillation system includes at least two cracking distillation units connected in parallel.

6. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 5, characterized in that, The continuous product distillation system also includes a first product receiving tank (21) located between the first product distillation column (17) and the product storage tank (27).

7. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 6, characterized in that, The first product distillation column (17), the first product distillation column condenser (18), the first pre-distillate tank (19), the first high-distillate tank (20) and the first product receiving tank (21) are combined to form a product distillation unit. The continuous product distillation system includes at least two product distillation units connected in parallel.

8. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 7, characterized in that, The fore-fraction recovery distillation system also includes a product receiving tank (35) located between the fore-fraction distillation column (30) and the product storage tank (27).

9. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to any one of claims 6-8, characterized in that, The number of product storage tanks (27) is at least two, connected in parallel.

10. The apparatus for continuous production of trifluoropropylmethylcyclotrisiloxane according to claim 9, characterized in that, The product storage tank (27) is connected to the product pump (28) at the bottom.

Citation Information

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