Equipment for improving output purity of methyltriacetoxysilane and preparation method

Abstract

The invention relates to the technical field of organic silicon compound purification, and mainly discloses equipment for improving the output purity of methyltriacetoxysilane and a preparation method, the equipment comprises a tower body, the tower body is internally provided with a mass transfer space; the tower plates are arranged in the mass transfer space and comprise buffer plates and drainage plates, and the buffer plates are located at the tops of the drainage plates; wherein lower leakage through holes are symmetrically formed in the drainage plate, and blocking plates for alternately blocking the lower leakage through holes are movably arranged at the bottom of the drainage plate; the problems that an existing rectifying tower plate is fixed in structure and cannot be adjusted according to material characteristics and working conditions, and the tower plate is prone to scaling and blocking and troublesome to clean and maintain are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of purification of organosilicon compounds, in particular to an apparatus and a preparation method for improving the purity of the output of methyltriacetoxysilane. Background Art

[0002] Methyltriacetoxysilane and its raw material acetic acid have high freezing points and are prone to solidification at normal or low temperatures. Continuous heat tracing is required during production, which not only greatly increases the energy cost, but also improves the operation complexity and safety risks. The performance of the product in low-temperature scenarios is also greatly affected, and it is urgent to lower the freezing point.

[0003] Methyltriethoxysilane is used in high-end fields and has extremely high purity requirements. However, existing purification methods are difficult to meet the standards, especially the problems of traditional distillation column trays are numerous. The structure of the traditional tray is fixed, and the hole opening rate and weir height cannot be adjusted according to the material characteristics and working conditions. The gas-liquid contact is single, and it is easy to have uneven gas-liquid distribution, serious liquid deviation and channeling, reduction of the mass transfer area, low mass transfer efficiency, and the product purity is affected. In terms of heat transfer, the heat exchange structure is simple and crude, and there is a lot of wasted heat energy. The operation flexibility is poor. When the working conditions change slightly, the separation ability drops suddenly. Moreover, due to the impurities in the raw materials and the complex reaction, the trays are prone to fouling and blockage, and the cleaning and maintenance are troublesome, which seriously affects the production efficiency and economic benefits. Summary of the Invention

[0004] Therefore, the technical problem to be solved by the present invention lies in that: the structure of the traditional distillation column tray is fixed, it cannot be adjusted according to the material characteristics and working conditions, and the tray is prone to fouling and blockage, and the cleaning and maintenance are troublesome.

[0005] The above technical problem is solved by the following technical solutions: The present invention provides an apparatus for improving the purity of the output of methyltriacetoxysilane, which includes a tower body having a mass transfer space therein; a plurality of groups of trays are arranged in the mass transfer space, including a buffer plate and a drainage plate, and the buffer plate is located on top of the drainage plate; wherein, downward leakage perforations are symmetrically formed in the drainage plate, a plugging plate for alternately plugging the downward leakage perforations is movably arranged at the bottom of the drainage plate, and; a dredging assembly is movably arranged in a plurality of groups of steam holes formed in the buffer plate and the drainage plate.

[0006] In a preferred embodiment of the apparatus for improving the purity of the output of methyltriacetoxysilane according to the present invention: side plates and guide plates are fixedly connected to the bottom of the drainage plate on both sides where the downward leakage perforations are formed, the side plates and the guide plates are fixedly connected to each other, and the drainage cavity formed by the two is communicated with the downward leakage perforations; overflow plates are symmetrically and vertically fixedly connected to the top of the drainage plate, and the overflow plates are located in the plane where the guide plates are located.

[0007] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: The steam holes are formed on the diversion plate between the overflow plates, and a first air cylinder is coaxially and fixedly connected to the top of the diversion plate at a position corresponding to the steam holes. The height of the first air cylinder is lower than the height of the overflow plate.

[0008] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: An embedded groove is formed in the inner wall of the guide plate close to the diversion cavity, and a fixed sliding groove is also communicated and formed on the side wall of the embedded groove close to the top opening of the leakage hole; A leakage prevention plate is slidably inserted into the guide plate. The leakage prevention plate includes a plugging section and a leakage prevention section fixedly connected to one side thereof. The plugging section is slidably inserted into the fixed sliding groove, and a first spring is fixedly connected between the plugging section and the bottom of the fixed sliding groove; The leakage prevention section is slidably inserted into the embedded groove.

[0009] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: A horizontal insertion hole is also formed on the side wall of the embedded groove at the end far from the fixed sliding groove, and a first inclined surface is formed at the edge of one end of the leakage prevention section close to the horizontal insertion hole.

[0010] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: The plugging plate includes main boards arranged symmetrically, and the main boards are fixedly connected by cross beams arranged symmetrically; Among them, the main boards are slidably inserted into the horizontal insertion holes and cooperate to block the diversion cavity. A second inclined surface is formed at the top of the edge of one side of the main board far from the cross beam, and the second inclined surface is in sliding contact with the first inclined surface; A connecting ear is fixedly connected to the inner wall of one cross beam close to the main board.

[0011] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: The dredging assembly includes a central connecting rod, a floating cylinder and a dredging ring. The floating cylinder and the dredging ring are respectively sleeved on the top and bottom ends of the central connecting rod, and a diversion column is coaxially and fixedly connected to the bottom end of the central connecting rod; Among them, the floating cylinder and the dredging ring can be inserted into the steam holes formed in the buffer plate and the diversion plate in cooperation; The floating cylinder and the central connecting rod are fixedly connected by a first docking block, and a first air hole is formed between the first docking blocks. The dredging ring and the central connecting rod are fixedly connected by a second docking block, and a second air hole is formed between the second docking blocks.

[0012] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: a water collecting groove is formed on the buffer plate, the steam hole array is formed in the water collecting groove, and a second air cylinder is coaxially and fixedly connected to the bottom of the water collecting groove corresponding to the steam hole; the outer edges of the top and bottom of the floating cylinder are respectively fixedly connected with a first abutting ring and a second abutting ring, and a plurality of groups of flow grooves are equidistantly formed on the outer wall of the floating cylinder near the first abutting ring. The first abutting ring and the second abutting ring are respectively located at the top and bottom of the second air cylinder; a floating bubble cover is further sleeved on the top of the first air cylinder, the central connecting rod slides through the floating bubble cover, a second spring is sleeved on the outer side of the central connecting rod, and the two ends of the second spring are respectively fixedly connected with the bottom floating bubble cover and the top first docking block. An air flow channel is formed between the inner wall of the floating bubble cover and the first air cylinder, and a plurality of groups of air grooves are equidistantly formed on the outer wall of the bottom end of the floating bubble cover.

[0013] In a preferred embodiment of the device for improving the output purity of methyltriacetoxysilane according to the present invention: a fixed shaft is fixedly connected on the axis of the tower body, the buffer plate is slidably sleeved outside the fixed shaft, and the drainage plate is fixedly sleeved outside the fixed shaft; a hydraulic cylinder is fixedly connected to the tower body, the output end of the hydraulic cylinder is fixedly connected with symmetrically arranged adjusting insertion rods, the adjusting insertion rods are movably inserted into the mass transfer space, the buffer plate is fixedly sleeved outside the adjusting insertion rods, and the drainage plate is slidably sleeved outside the adjusting insertion rods; an adjusting sleeve is further fixedly connected to the adjusting insertion rods, hinge blocks are symmetrically and fixedly connected to both ends of the adjusting sleeve, a hinge rod is rotatably connected between the hinge blocks, and the other end of the hinge rod is vertically fixedly connected with an insertion rod, and the insertion rod can be rotatably inserted into the connecting ear for cooperation.

[0014] The above technical problems are also solved by the following technical solution: a preparation method for improving the output purity of methyltriacetoxysilane, which is based on the above device for improving the output purity of methyltriacetoxysilane, further includes the following steps: the vortex-mixed material is sent into the fixed tower plate at the lower layer of the tower body, the bottom reboiler heats by means of a nano-coating, the temperature is adjusted according to the real-time instrument monitoring, so that the material is vaporized to form a gas phase, and the gas phase and the liquid phase perform preliminary mass transfer on the lower tower plate; the rising gas meets the movable tower plate at the upper layer, and according to the mass transfer situation of the material, the plate spacing between the buffer plate and the drainage plate is adjusted to strengthen the mass transfer; a multi-parameter sensor collects data in the mass transfer space and gives it to the processing system, and accordingly adjusts the reflux ratio, and the buffer plate is dynamically adjusted according to the mass transfer effect; a molecular sieve condensation device is used at the top of the tower body to collect high-purity products, supercritical fluid extraction is used at the bottom of the tower to treat impurities, and the plate spacing of the tower plate is adjusted in real time according to the change of the material.

[0015] The beneficial effects of the present invention are as follows: The plate spacing between the buffer plate and the drainage plate can be controlled by a hydraulic cylinder. During the rectification process, when the mass transfer resistance encountered by substances during the transfer between the gas phase and the liquid phase is large, the plate spacing between the buffer plate and the drainage plate can be increased, the flow path of the liquid phase can be increased, and the contact time between the gas phase and the liquid phase can be increased, thereby greatly improving the mass transfer efficiency and purifying methyltriacetoxysilane more efficiently.

[0016] At the same time, during the continuous change of the plate spacing between the buffer plate and the drainage plate, the dredging component can clean the scale in the steam holes, dredge the steam holes, and prevent scale blockage from affecting the mass transfer efficiency between the gas phase and the liquid phase. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments of the present invention will be briefly introduced below. Obviously, the drawings described below only relate to some embodiments of the present invention and do not limit the present invention. Among them: Figure 1 Shows an overall cross-sectional view of the device that can improve the output purity of methyltriacetoxysilane; Figure 2 Shows an installation schematic diagram of the tray and the dredging component of the device that can improve the output purity of methyltriacetoxysilane; Figure 3 Shows a structural diagram of the drainage plate of the device that can improve the output purity of methyltriacetoxysilane; Figure 4 Shows a cross-sectional view of the drainage plate of the device that can improve the output purity of methyltriacetoxysilane; Figure 5 Shows an installation schematic diagram of the plugging plate of the device that can improve the output purity of methyltriacetoxysilane; Figure 6 Shows a cross-sectional view of the dredging component of the device that can improve the output purity of methyltriacetoxysilane; Figure 7 Shows a cross-sectional view of the tray of the device that can improve the output purity of methyltriacetoxysilane; Figure 8 Shows an installation schematic diagram of the floating bubble cap of the device that can improve the output purity of methyltriacetoxysilane; Figure 9 Shows a structural diagram of the tower body of the device that can improve the output purity of methyltriacetoxysilane; Figure 10 Shows a schematic diagram of the liquid phase flow path of the device that can improve the output purity of methyltriacetoxysilane. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0018] To enable those skilled in the art to better understand the present invention, the present invention will be further described in detail below in conjunction with specific embodiments and the accompanying drawings.

[0019] The terms used in the present invention are those general terms currently widely used in the art in consideration of the functions of the present invention, but these terms may vary according to the intentions of those of ordinary skill in the art, precedents, or new technologies in the art. In addition, specific terms may be selected by the applicant, and in such cases, their detailed meanings will be described in the detailed description of the present invention. Therefore, the terms used in the specification should not be understood as simple names, but based on the meanings of the terms and the overall description of the present invention.

[0020] Referring to Figures 1 to 10 , this embodiment provides a device that can improve the output purity of methyltriacetoxysilane, which includes a tower body 100, and a mass transfer space A is provided inside the tower body 100.

[0021] Among them, the tower body 100 is preferably an upright cylindrical tank made of carbon steel, the internal mass transfer space A is the internal cavity of the tank body, the top and bottom of the tower body 100 are sealed, and the mass transfer space A is a sealed space.

[0022] Trays 200, several groups are arranged in the mass transfer space A, including a buffer plate 201 and a drainage plate 202, and the buffer plate 201 is located at the top of the drainage plate 202.

[0023] Among them, downward leakage perforations B are symmetrically opened in the drainage plate 202, and a blocking plate 203 that alternately blocks the downward leakage perforations B is movably arranged at the bottom of the drainage plate 202.

[0024] Furthermore, each group of trays 200 includes a buffer plate 201, a drainage plate 202, and a blocking plate 203. The buffer plate 201 can move up and down in the mass transfer space A to actively change the plate spacing between the buffer plate 201 and the drainage plate 202.

[0025] Furthermore, the downward leakage perforations B are symmetrically opened on the drainage plate 202 for the liquid phase to pass through the downward leakage perforations B and flow onto the next-level buffer plate 201, and the blocking plate 203 can always maintain a group of downward leakage perforations B on the drainage plate 202 in a blocked state.

[0026] Referring to Figure 10 , in this solution, the positions of the downward leakage perforations B in the open state in adjacent two groups of drainage plates 202 are opposite, so that the liquid phase flows freely left and right.

[0027] Furthermore, there is a maximum distance and a minimum distance between the buffer plate 201 and the drainage plate 202. When the distance between the buffer plate 201 and the drainage plate 202 is adjusted from the minimum distance to the maximum distance, or from the maximum distance to the minimum distance, the plugging plate 203 will change the corresponding leaking perforation B to be plugged, so as to change the position where the liquid phase flows downward.

[0028] The dredging assembly 300 is movably arranged in a plurality of groups of steam holes C formed in the buffer plate 201 and the drainage plate 202.

[0029] During the process of changing the plate distance between the buffer plate 201 and the drainage plate 202, the dredging assembly 300 will clean the possible scale existing inside the steam holes C to prevent the steam holes C through which the gas phase passes from being blocked.

[0030] As an alternative embodiment, side plates 202a and guide plates 202b are fixedly connected to the bottom of the drainage plate 202 on both sides of the leaking perforation B. The side plates 202a and the guide plates 202b are fixedly connected to each other, and the drainage cavity D formed by the two is communicated with the leaking perforation B.

[0031] Among them, the buffer plate 201 and the drainage plate 202 preferably adopt a circular plate structure, and their outer diameters are equal to the inner diameter of the inner cavity of the tower body 100, ensuring that the buffer plate 201 and the drainage plate 202 can completely seal the mass transfer space A radially to form a plurality of relatively independent mass transfer chambers.

[0032] Further, the side plates 202a preferably adopt mutually parallel plates, the guide plates 202b are rectangular plates, and the two ends of the side plates 202a and the guide plates 202b are fixedly connected to each other. In this embodiment, preferably, an integrated casting method is adopted to hermetically fix the side plates 202a and the guide plates 202b below the leaking perforation B to form the drainage cavity D. When the liquid phase flow rate is small, it can flow smoothly along the guide plates 202b to the surface of the next-level buffer plate 201. When the liquid phase flow rate becomes large, the drainage cavity D will be filled with the liquid phase.

[0033] Overflow plates 202c are symmetrically and vertically fixedly connected to the top of the drainage plate 202, and the overflow plates 202c are located in the plane where the guide plates 202b are located.

[0034] After the liquid phase flows to the surface of the drainage plate 202, it will be stored between the overflow plates 202c until the liquid level is higher than the overflow plates 202c, and then it can enter the surface of the next-level buffer plate 201 from the opened side leaking perforation B and the drainage cavity D.

[0035] The steam holes C are opened on the diversion plate 202 between the overflow plates 202c. At the top of the diversion plate 202 corresponding to the steam holes C, a first air cylinder C1 is coaxially and fixedly connected. The height of the first air cylinder C1 is lower than the height of the overflow plate 202c. When the gas phase rises from below, it can ensure that the liquid phase covers the air outlet at the top of the first air cylinder C1. At this time, after the gas phase passes through the liquid phase, bubbles are formed in the liquid phase, continue to rise, and are discharged from above the liquid surface.

[0036] Referring to Figure 4 , an embedded groove 202b-1 is opened on the inner wall of the guide plate 202b close to the diversion cavity D. A fixed sliding groove 202b-2 is also communicated and opened on the side wall of the embedded groove 202b-1 close to the top opening of the lower leakage perforation B.

[0037] A leak-proof plate 202b-3 is slidably inserted into the guide plate 202b. The leak-proof plate 202b-3 includes an insertion section 202b-3a and a leak-proof section 202b-3b fixedly connected to one side thereof. The insertion section 202b-3a is slidably inserted into the fixed sliding groove 202b-2, and a first spring T1 is also fixedly connected between the insertion section 202b-3a and the bottom of the fixed sliding groove 202b-2.

[0038] The leak-proof section 202b-3b is slidably inserted into the embedded groove 202b-1.

[0039] A horizontal insertion hole 202b-1a is also opened on the side wall of the embedded groove 202b-1 at the end far from the fixed sliding groove 202b-2. A first inclined surface X1 is opened at the edge of one end of the leak-proof section 202b-3b close to the horizontal insertion hole 202b-1a.

[0040] During use, under the action of the elastic force of the first spring T1 and the self-gravity of the leak-proof plate 202b-3, the lower end of the leak-proof section 202b-3b will closely adhere to the bottom of the lower groove of the embedded groove 202b-1, and the whole leak-proof plate 202b-3 will block the horizontal insertion hole 202b-1a.

[0041] The plugging plate 203 includes main plates 203a arranged symmetrically. The main plates 203a are fixedly connected by cross beams 203b arranged symmetrically.

[0042] Among them, the main plate 203a is slidably inserted into the horizontal insertion hole 202b-1a and cooperates to block the diversion cavity D. A second inclined surface X2 is opened at the top edge of one side of the main plate 203a far from the cross beam 203b. The second inclined surface X2 is in sliding contact with the first inclined surface X1.

[0043] Referring to Figure 4 and Figure 5, Further, the lower end opening of the drainage cavity D on the right side in the open state, if it needs to be closed, switch to the left drainage cavity D being open. At this time, the plugging plate 203 moves to the right, the left main plate 203a is pushed out from the left drainage cavity D, and the right main plate 203a starts to contact the leak-proof plate 202b-3. At this time, the second inclined plane X2 slides against the first inclined plane X1, slightly pushing up the leak-proof plate 202b-3, and the horizontal insertion hole 202b-1a is completely opened.

[0044] Further, the right main plate 203a is gradually inserted into the right drainage cavity D to completely block the drainage cavity D. At the same time, after the left main plate 203a completely exits the left drainage cavity D, the left leak-proof plate 202b-3 on the left is inserted downward to seal the inner wall of the left guide plate 202b of the vacant space.

[0045] A connecting ear 203b-1 is also fixedly connected to the inner wall of one side cross beam 203b close to the main plate 203a.

[0046] Further, referring to Figure 6 and Figure 7 , the dredging component 300 includes a central connecting rod 301, a floating cylinder 302 and a dredging ring 303. The floating cylinder 302 and the dredging ring 303 are respectively sleeved on the top end and the bottom end of the central connecting rod 301. A drainage column 304 is also coaxially and fixedly connected to the bottom end of the central connecting rod 301.

[0047] Among them, the floating cylinder 302 and the dredging ring 303 can be cooperatively inserted into the steam holes C opened in the buffer plate 201 and the drainage plate 202.

[0048] The floating cylinder 302 and the central connecting rod 301 are fixedly connected through a first docking block 301a, and a first air hole 301a-1 is formed between the first docking blocks 301a. The dredging ring 303 and the central connecting rod 301 are fixedly connected through a second docking block 301b, and a second air hole 301a-2 is formed between the second docking blocks 301b.

[0049] During the use process, the gas phase rises from bottom to top. First, it passes through the steam hole C opened on the drainage plate 202, moves to the main mass transfer space between the drainage plate 202 and the buffer plate 201, and then continues to rise. After passing through the first air hole 301a-1, it rises above the buffer plate 201.

[0050] A water collecting tank 201a is opened on the buffer plate 201. The steam holes C are arranged in an array in the water collecting tank 201a. A second air cylinder C2 is coaxially and fixedly connected to the bottom of the water collecting tank 201a corresponding to the steam hole C.

[0051] At the top and bottom outer edges of the floating cylinder 302, a first abutting ring 302a and a second abutting ring 302b are fixedly connected respectively. A plurality of groups of flow grooves 302c are equidistantly arranged on the circumferential outer wall near the first abutting ring 302a. The first abutting ring 302a and the second abutting ring 302b are respectively located at the top and bottom of the second air cylinder C2.

[0052] A floating bubble cover 204 is also sleeved on the top of the first air cylinder C1. The central connecting rod 301 slidably passes through the floating bubble cover 204. A second spring T2 is sleeved outside the central connecting rod 301. The two ends of the second spring T2 are respectively fixedly connected to the bottom floating bubble cover 204 and the top first docking block 301a. In this embodiment, the second spring T2 is softer and has a smaller elastic coefficient. However, whether the plate spacing is at the maximum spacing or the minimum spacing, the second spring T2 can give the floating bubble cover 204 a more appropriate thrust to prevent it from being lifted too much under the influence of the upward thrust of the gas phase. An air flow channel E is formed between the inner wall of the floating bubble cover 204 and the first air cylinder C1. A plurality of groups of air grooves 204a are equidistantly arranged on the circumferential outer wall at the bottom end of the floating bubble cover 204.

[0053] Refer to Figure 7 , at this time, the maximum spacing exists between the buffer plate 201 and the drainage plate 202. This mode is applicable to the situation of high-viscosity materials or high impurity content, slow mass transfer rate, or insufficient gas-liquid contact time.

[0054] When the mass transfer driving force is large and the gas phase flow rate is too fast, etc., the buffer plate 201 can be moved downward to switch to the minimum spacing mode to improve the mass transfer efficiency.

[0055] Furthermore, during the use process, the liquid phase falls from above and first lands on the buffer plate 201. Since the water collecting tank 201a and the second air cylinder C2 are arranged in the middle of the buffer plate 201, the liquid phase will leak downward from the middle of the buffer plate 201 and fall onto the plate surface of the drainage plate 202 between the overflow plates 202c, and then fall from one side of the drainage cavity D.

[0056] During the process of switching the plate spacing from the maximum spacing to the minimum spacing, the buffer plate 201 moves downward, quickly pushes the central connecting rod 301 downward through the second abutting ring 302b, and synchronously drives the dredging ring 303 to be inserted into the first air cylinder C1. When the minimum spacing is reached, the dredging ring 303 will pass through and clean the inner cavity of the first air cylinder C1 and reach the bottom of the drainage plate 202. At the same time, the height difference between the top of the floating cylinder 302 connected with the first abutting ring 302a and the plate surface of the buffer plate 201 becomes larger, exposing the flow grooves 302c. The liquid phase enters the floating cylinder 302 from the flow grooves 302c and falls from the first air hole 301a-1.

[0057] Furthermore, during this process, the floating bubble cover 204 can always cover the first air cylinder C1. The gas phase flows along the air flow channel E, forms water bubbles, and is discharged from the air grooves 204a.

[0058] During the process of the plate spacing switching from the minimum spacing to the maximum spacing, the buffer plate 201 moves upward, driving the overall lifting of the dredging assembly 300 through the first abutting ring 302a. The dredging ring 303 will pass through and clean the inner cavity of the first air cylinder C1 and reach the top of the drainage plate 202.

[0059] A fixed shaft 101 is fixedly connected on the axis of the tower body 100. The buffer plate 201 is slidably sleeved outside the fixed shaft 101, and the drainage plate 202 is fixedly sleeved outside the fixed shaft 101.

[0060] The tower body 100 is fixedly connected with a hydraulic cylinder 102. The output end of the hydraulic cylinder 102 is fixedly connected with symmetrically arranged adjusting insertion rods 102a. The adjusting insertion rods 102a are movably inserted into the mass transfer space A. The buffer plate 201 is fixedly sleeved outside the adjusting insertion rods 102a, and the drainage plate 202 is movably sleeved outside the adjusting insertion rods 102a.

[0061] An adjusting sleeve 103 is also fixedly connected to the adjusting insertion rod 102a. Symmetrically arranged hinge blocks 103a are fixedly connected to both ends of the adjusting sleeve 103. A hinge rod 103b is rotatably connected between the hinge blocks 103a. The other end of the hinge rod 103b is vertically fixedly connected with an insertion rod 103c, and the insertion rod 103c can be rotatably inserted into the connecting ear 203b-1 for cooperation.

[0062] In summary, in this embodiment, the hydraulic cylinder 102 provides driving force to drive the movement of the adjusting insertion rod 102a, and the adjusting insertion rod 102a drives the buffer plate 201 and the adjusting sleeve 103 to move up and down. The adjusting sleeve 103 can push the sealing plate 203 through the hinge rod 103b, while adjusting the plate spacing, it can also change the liquid phase flow path and improve the mass transfer efficiency.

[0063] A preparation method for improving the output purity of methyltriacetoxysilane, based on the above-mentioned equipment for improving the output purity of methyltriacetoxysilane, further includes the following steps: After the materials are vortex-mixed, they are sent to the lower fixed tower plate of the tower body 100. The bottom reboiler heats by means of a nano-coating, and the temperature is adjusted according to the real-time instrument monitoring, so that the materials are vaporized to form a gas phase, and the gas phase undergoes preliminary mass transfer with the liquid phase on the lower tower plate.

[0064] When the rising gas meets the upper movable tower plate 200, according to the mass transfer situation of the materials, the plate spacing between the buffer plate 201 and the drainage plate 202 is adjusted to strengthen the mass transfer.

[0065] The multi-parameter sensor collects the data in the mass transfer space A and gives it to the processing system, and accordingly adjusts the reflux ratio, and the buffer plate 201 is dynamically adjusted according to the mass transfer effect.

[0066] At the top of the tower body 100, a molecular sieve condensation device is used to collect high-purity products, and at the bottom of the tower, supercritical fluid extraction is used to treat impurities. The tray 200 adjusts the tray spacing in real time according to the change of the material.

[0067] Specifically, an Agilent 7890B~5977B gas chromatography-mass spectrometry instrument is used to scan the mass range of 10~1050 amu to accurately identify the components of the material. It is paired with a Shimadzu LC~2030C3D liquid chromatography instrument and a C18 reversed-phase column to analyze the content of each component, and the detection limit reaches the nanogram level. With the help of a high-precision densitometer, a rotational viscometer and a differential scanning calorimeter, the density, viscosity and boiling points of each component of the material are obtained, and the process parameters such as the temperature and pressure of each tower section of the distillation column are set accordingly.

[0068] Furthermore, for the material premixing and feeding device, its eddy current generator is driven by a variable-frequency motor, and the rotation speed is adjustable from 0 to 3000 r / min. According to the feedback of the angle sensor, the blade angle is accurately adjusted to change from 0 to 90°. For materials that are prone to stratification, the feeding speed is increased to 50~100 L / min, the mixing time is extended to 10~15 min, and the feeding ratio is reasonably set according to the content of methyltriacetoxysilane to ensure sufficient mixing. Furthermore, a Milton Roy ProMinent electromagnetic diaphragm metering pump is used, with a flow regulation range of 0~500 L / h and an accuracy of ±1%. Combined with the feedback of a mass flowmeter, the material is stably transported to the lower fixed tray of the tower body 100, and the feeding pressure is maintained at 0.2~0.5 MPa. The bottom reboiler is coated with a silicon carbide nano-coating and equipped with a 50~100 kW electric heating element, and the heating power is regulated by a thyristor power regulator.

[0069] Through a armored thermocouple temperature sensor and a near-infrared spectroscopy composition analyzer, according to the changes in temperature and composition, the heating power is adjusted by a PLC system to promote the vaporization of the material, and the initial gas-liquid mass transfer is realized on the lower tray. At this time, the tray temperature is 120~150 °C and the pressure is 0.05~0.1 MPa.

[0070] Still further, the upper movable tray 200 is composed of a buffer plate 201 and a drainage plate 202. The stroke of the push rod of the hydraulic cylinder 102 at the top of the tower is 0~200 mm, the positioning accuracy is ±0.1 mm, and the response time is less than 0.1 s. The gas-liquid phase parameters are monitored through a pressure sensor and a vortex flowmeter. When the mass transfer resistance is large, the tray spacing is reduced to 20~50 mm; when the gas-liquid contact time is short, it is increased to 80~120 mm. The mass transfer can also be enhanced by using turbulence elements and optimizing the drainage plate, etc.

[0071] Furthermore, a multi-parameter sensor matrix is installed at the position between each group of trays 200, and the data is transmitted to a processing system developed based on Python through a ZigBee module at a frequency of 10 Hz. The system uses a deep neural network algorithm and a support vector machine model to calculate the optimal reflux ratio according to the preset target of purity ≥ 99.5% and the energy consumption strategy, and controls a pneumatic diaphragm regulating valve with a flow regulation range of 0 - 100 m³ / h and an accuracy of ±1%. At the same time, the position of the buffer plate 201 is dynamically adjusted according to the mass transfer effect, with each adjustment being 5 - 10 mm.

[0072] The molecular sieve condensation device at the top of the tower body 100 uses a zeolite molecular sieve membrane with a pore size of 0.3 - 0.5 nm to screen the product. After passing through a shell-and-tube condenser with a heat exchange area of 10 - 20 m², the temperature is controlled at 15 - 25 °C by circulating water for condensation and collection.

[0073] Furthermore, the collection tank is switched according to the liquid level and flow sensors. The bottom liquid phase of the tower is sent to a supercritical fluid extraction device, using carbon dioxide as the extraction agent, at a temperature of 35 - 40 °C and a pressure of 8 - 10 MPa. The valuable components are separated and recycled for further purification, and the impurities are discharged up to standard. The processing system evaluates every 10 - 15 minutes based on the tray sensor data. If the concentration fluctuation of methyltriacetoxysilane exceeds ±0.5%, the tray spacing is adjusted to ensure the effect.

[0074] Finally, it should be pointed out that the methods and devices described in detail above are only examples, and those skilled in the art can modify these examples in different ways as long as they do not depart from the scope of the present invention.

Claims

1. An apparatus for improving the output purity of methyltriacetoxysilane, characterized in that: including, a tower body (100) with a mass transfer space (A) therein; a plurality of groups of tower trays (200) are arranged in the mass transfer space (A), including a buffer plate (201) and a drainage plate (202), and the buffer plate (201) is located at the top of the drainage plate (202); wherein, downward leakage perforations (B) are symmetrically formed in the drainage plate (202), and a plugging plate (203) for alternately plugging the downward leakage perforations (B) is movably arranged at the bottom of the drainage plate (202), and; a dredging assembly (300) is movably arranged in a plurality of groups of steam holes (C) formed in the buffer plate (201) and the drainage plate (202).

2. The device for improving the output purity of methyltriacetoxysilane according to claim 1, characterized in that: Side plates (202a) and guide plates (202b) are fixedly connected to the bottom of the drainage plate (202) on both sides of the downward leakage perforation (B). The side plates (202a) and the guide plates (202b) are fixedly connected to each other, and a drainage cavity (D) formed by the two is communicated with the downward leakage perforation (B); Overflow plates (202c) are symmetrically and vertically fixedly connected to the top of the drainage plate (202), and the overflow plates (202c) are located in the plane where the guide plates (202b) are located.

3. The device for improving the output purity of methyltriacetoxysilane according to claim 2, characterized in that: The steam holes (C) are formed in the drainage plate (202) between the overflow plates (202c), and a first air cylinder (C1) is coaxially and fixedly connected to the top of the drainage plate (202) at a position corresponding to the steam holes (C). The height of the first air cylinder (C1) is lower than the height of the overflow plates (202c).

4. The device for improving the output purity of methyltriacetoxysilane according to claim 3, characterized in that: An embedded groove (202b-1) is formed in the inner wall of the guide plate (202b) close to the drainage cavity (D), and a fixed sliding groove (202b-2) is also communicated and formed in the side wall of the embedded groove (202b-1) close to the top opening of the downward leakage perforation (B); A leak-proof plate (202b-3) is slidably inserted into the guide plate (202b). The leak-proof plate (202b-3) includes an insertion section (202b-3a) and a leak-proof section (202b-3b) fixedly connected to one side thereof. The insertion section (202b-3a) is slidably inserted into the fixed sliding groove (202b-2), and a first spring (T1) is also fixedly connected between the insertion section (202b-3a) and the bottom of the fixed sliding groove (202b-2); The leak-proof section (202b-3b) is slidably inserted into the embedded groove (202b-1).

5. The device for improving the output purity of methyltriacetoxysilane according to claim 4, characterized in that: A horizontal insertion hole (202b-1a) is further formed in the side wall of the embedded groove (202b-1) at one end far from the fixed sliding groove (202b-2), and a first inclined surface (X1) is formed at the edge of one end of the leak-proof section (202b-3b) close to the horizontal insertion hole (202b-1a).

6. The device for improving the output purity of methyltriacetoxysilane according to claim 5, wherein: The plugging plate (203) includes main boards (203a) arranged symmetrically, and the main boards (203a) are fixedly connected by cross beams (203b) arranged symmetrically; Among them, the main board (203a) is slidably inserted into the horizontal jack (202b-1a) and cooperates to block the drainage cavity (D). A second inclined surface (X2) is provided at the top of the edge of the main board (203a) on the side away from the cross beam (203b), and the second inclined surface (X2) is in sliding contact with the first inclined surface (X1); On one side, a connecting ear (203b-1) is fixedly connected to the inner wall of the cross beam (203b) close to the main board (203a).

7. The device for improving the output purity of methyltriacetoxysilane according to any one of claims 3 to 6, characterized in that: The dredging component (300) includes a central connecting rod (301), a floating cylinder (302) and a dredging ring (303). The floating cylinder (302) and the dredging ring (303) are respectively sleeved on the top end and the bottom end of the central connecting rod (301), and a drainage column (304) is coaxially and fixedly connected to the bottom end of the central connecting rod (301); Among them, the floating cylinder (302) and the dredging ring (303) can be cooperatively inserted into the steam holes (C) provided in the buffer plate (201) and the drainage plate (202); The floating cylinder (302) and the central connecting rod (301) are fixedly connected through a first docking block (301a), and a first air hole (301a-1) is formed between the first docking blocks (301a). The dredging ring (303) and the central connecting rod (301) are fixedly connected through a second docking block (301b), and a second air hole (301a-2) is formed between the second docking blocks (301b).

8. The device for improving the output purity of methyltriacetoxysilane according to claim 7, characterized in that: A water collecting tank (201a) is provided on the buffer plate (201), the steam holes (C) are arranged in an array in the water collecting tank (201a), and a second air cylinder (C2) is coaxially and fixedly connected to the bottom of the water collecting tank (201a) corresponding to the steam holes (C); First abutting rings (302a) and second abutting rings (302b) are respectively fixedly connected to the outer edges of the top end and the bottom end of the floating cylinder (302). A plurality of groups of flow grooves (302c) are equidistantly provided on the circumferential outer wall of the floating cylinder (302) close to the first abutting ring (302a). The first abutting rings (302a) and the second abutting rings (302b) are respectively located at the top end and the bottom end of the second air cylinder (C2); A floating bubble cover (204) is further sleeved on the top of the first air cylinder (C1). The central connecting rod (301) slides through the floating bubble cover (204). A second spring (T2) is sleeved on the central connecting rod (301). The two ends of the second spring (T2) are respectively fixedly connected to the bottom floating bubble cover (204) and the top first docking block (301a). An air flow channel (E) is formed between the inner wall of the floating bubble cover (204) and the first air cylinder (C1). A plurality of groups of air grooves (204a) are equidistantly provided on the circumferential outer wall of the bottom end of the floating bubble cover (204).

9. The device for improving the output purity of methyltriacetoxysilane according to claim 6, characterized in that: A fixed shaft (101) is fixedly connected on the axis of the tower body (100). The buffer plate (201) is slidably sleeved outside the fixed shaft (101), and the drainage plate (202) is fixedly sleeved outside the fixed shaft (101); The tower body (100) is fixedly connected with a hydraulic cylinder (102). The output end of the hydraulic cylinder (102) is fixedly connected with symmetrically arranged adjusting insertion rods (102a). The adjusting insertion rods (102a) are movably inserted into the mass transfer space (A). The buffer plate (201) is fixedly sleeved outside the adjusting insertion rods (102a). The drainage plate (202) is movably sleeved outside the adjusting insertion rods (102a). An adjusting kit (103) is further fixedly connected to the adjusting insertion rods (102a). Symmetrically arranged hinge blocks (103a) are fixedly connected to both ends of the adjusting kit (103). A hinge rod (103b) is rotatably connected between the hinge blocks (103a). The other end of the hinge rod (103b) is vertically fixedly connected with an insertion rod (103c), and the insertion rod (103c) can be rotatably inserted into the connecting ear (203b-1) in cooperation.

10. A preparation method capable of improving the output purity of methyltriacetoxysilane, characterized in that: Based on the equipment for improving the output purity of methyltriacetoxysilane as described in any one of claims 1 to 9, the following steps are further included. After the eddy current mixes the materials evenly, they are sent to the fixed tower plate at the lower layer of the tower body (100). The bottom reboiler heats by means of a nano-coating. The temperature is adjusted according to the real-time instrument monitoring, so that the materials are vaporized to form a gas phase. The gas phase and the liquid phase perform preliminary mass transfer on the lower tower plate. When the rising gas meets the upper movable tower plate (200), according to the mass transfer situation of the materials, the plate spacing between the buffer plate (201) and the drainage plate (202) is adjusted to strengthen the mass transfer. The multi-parameter sensor collects the data in the mass transfer space (A) and gives it to the processing system. Accordingly, the reflux ratio is adjusted, and the buffer plate (201) is dynamically adjusted according to the mass transfer effect. At the top of the tower body (100), a molecular sieve condensation device is used to collect high-purity products. At the bottom of the tower, supercritical fluid extraction is used to treat impurities. The tower plate (200) adjusts the plate spacing in real time according to the change of the materials.

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