Centrifugal filtration method for continuously preparing silane coupling agent

Abstract

The invention discloses a centrifugal filtration method for continuously preparing a silane coupling agent, and belongs to the technical field of silane coupling agents.According to the centrifugal filtration method for continuously preparing the silane coupling agent.According to the centrifugal filtration method for continuously preparing the silane coupling agent, the steps of mixing and reacting can be conducted at the same time during centrifugal treatment, the production efficiency is greatly improved, and the production cost is reduced. According to the mixing centrifugal equipment, the mixing mechanism and the centrifugal mechanism are arranged, the mixing function and the centrifugal function are integrated, the number of equipment needed on a production line is reduced, the production space is saved, the mixing function and the centrifugal function are tightly combined, so that materials can be continuously treated in the mixing centrifugal equipment, midway transfer is not needed, and the production efficiency is improved. And the energy consumption and the time cost during transferring are saved, and the production efficiency is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of silane coupling agent generation, and in particular relates to a centrifugal filtration method for continuously preparing a silane coupling agent. Background Art

[0002] In the field of chemical industry, silane coupling agent, as an important organosilicon compound, is widely used in material modification, enhancing adhesion and improving the performance of composite materials. The research and optimization of its preparation method has always been a hot topic in the industry. Traditionally, the preparation of silane coupling agent mostly adopts intermittent reaction process, which has problems such as low production efficiency and uneven product purity, and it is difficult to meet the needs of large-scale industrial production. In recent years, with the rise of continuous production technology, it has become an urgent need to develop an efficient and continuous preparation process for silane coupling agent.

[0003] In the prior art, although there have been attempts to prepare silane coupling agents by continuous means, these methods often focus on the optimization of reaction conditions or the use of specific catalysts, but pay insufficient attention to the separation and purification of the mixture after the reaction.

[0004] Specifically, the traditional method of preparing silane coupling agents cannot complete continuous material heating, stirring and centrifugation through the preparation equipment, which increases the energy consumption and time cost of materials during transportation and needs to be improved. Summary of the invention

[0005] The object of the present invention is to provide a centrifugal filtration method for continuously preparing a silane coupling agent, which is used to solve the technical problem that the traditional centrifugal filtration method for continuously preparing a silane coupling agent in the prior art cannot complete continuous material heating, stirring and centrifugation through preparation equipment, thereby increasing the energy consumption and time cost of the material during transportation.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] The centrifugal filtration method for continuously preparing a silane coupling agent comprises the following steps: step 1, transporting a catalyst to a first material tank through a catalyst pipeline, transporting olefins to the first material tank through an olefin pipeline, and mixing the two uniformly through a stirrer to obtain olefins containing catalysts; step 2, transporting the olefins containing catalysts in the first material tank to a mixing centrifugal device through a first delivery pump, and transporting the hydrosilane in the second material tank to the mixing centrifugal device through a second delivery pump; step 3, a mixing mechanism in the mixing centrifugal device heats the olefins containing catalysts and the hydrosilane to a reaction temperature, and then heats the olefins containing catalysts and the hydrosilane to a reaction temperature. Stirring to allow the olefins containing the catalyst and the hydrosilane to react in the mixing mechanism for 2-4 hours; step 4, transporting the reaction product in the mixing mechanism to the centrifugal mechanism in the mixing centrifugal device; repeating steps 1 to 3 to allow new olefins containing the catalyst and the hydrosilane to react in the mixing mechanism; step 5, centrifuging the reaction product through the centrifugal mechanism to obtain a filtrate; step 6, starting the third delivery pump to extract the filtrate in the centrifugal mechanism, and transporting the filtrate to a vacuum reaction distillation tower for distillation separation to obtain a high-purity silane coupling agent; step 7, transporting the high-purity silane coupling agent to a product storage tank for storage.

[0008] Preferably, the mixing centrifugal device includes: a mixing mechanism for heating and stirring olefins and hydrosilane containing catalysts; a centrifugal mechanism located below the mixing mechanism, for receiving the post-reaction products discharged from the mixing mechanism and centrifuging the post-reaction products.

[0009] Preferably, the mixing mechanism includes: a mixing barrel; a connecting pipe installed at the bottom of the mixing barrel; a first valve installed on the connecting pipe; a first delivery pipe installed on the side of the mixing barrel, the other end of which is connected to the delivery pipe of a first delivery pump; a second delivery pipe installed on the side of the mixing barrel, the other end of which is connected to the delivery pipe of a second delivery pump; a heating sleeve mounted on the mixing barrel for heating the material in the mixing barrel; and a stirring assembly for stirring the material in the mixing barrel.

[0010] Preferably, the stirring assembly comprises: a shaft rod, which passes through the mixing barrel and is rotatably connected to the mixing barrel; and a plurality of stirring rods, which are all located in the mixing barrel and fixedly connected to the shaft rod.

[0011] Preferably, the centrifugal mechanism includes: a fixed cylinder, installed directly below the mixing cylinder, and the lower end of the connecting pipe passes through the top surface of the fixed cylinder; a discharge pipe, installed on the bottom surface of the fixed cylinder; a second valve, fixedly sleeved on the discharge pipe; a liquid discharge pipe, installed on the bottom surface of the fixed cylinder and connected to the suction pipe of the third delivery pump; a discharge pipe, slidably connected to the connecting pipe; a centrifugal assembly; and a driving assembly, used to drive the centrifugal assembly to rotate.

[0012] Preferably, the centrifugal assembly comprises: a centrifugal cylinder rotatably mounted in the fixed cylinder, wherein the lower end of the connecting tube is located in the centrifugal cylinder; and an outer gear ring fixedly sleeved on a side surface of the centrifugal cylinder.

[0013] Preferably, the driving assembly includes: a dual-axis motor installed on the top surface of the fixed cylinder, whose lower power output shaft extends into the fixed cylinder and is rotatably connected to the fixed cylinder; a gear installed on the lower power output shaft of the dual-axis motor and meshingly connected with the outer gear ring; a reducer installed on the mixing cylinder, whose input shaft is fixedly connected to the upper power output shaft of the dual-axis motor; and a transmission belt mounted on the output shaft and shaft rod of the reducer.

[0014] Preferably, the centrifugal mechanism also includes a tube adjusting assembly, which includes: a reciprocating screw, which passes through the top surface of the fixed cylinder and is rotatably connected to the fixed cylinder, and its upper end is fixedly connected to the lower end of the shaft rod; a movable seat, which is sleeved on the reciprocating screw; and a connecting plate, which is fixedly sleeved on the movable seat and fixedly connected to the discharge pipe.

[0015] Preferably, the hybrid centrifugal device also includes a centrifugal control system, which includes: a data acquisition module, which is used to collect comprehensive data information of the hybrid centrifugal device, wherein the comprehensive data information includes the density of the reaction product in the centrifuge cylinder, the temperature of the reaction product, the viscosity of the reaction product and the weight of the reaction product; a data analysis module, which generates a speed influence coefficient according to the comprehensive data information, and generates a corresponding centrifugal speed level according to the speed influence coefficient; a data acquisition module, which is used to collect a historical training data set of the hybrid centrifugal device, the historical training data set includes comprehensive speed influence data and centrifugal time; the comprehensive speed influence data includes comprehensive data information and speed data of the dual-axis motor; a time prediction module, which trains a machine learning model for predicting the centrifugal time based on the historical training data set, collects real-time comprehensive speed influence data, and inputs it into the trained machine learning model to predict the centrifugal time.

[0016] Preferably, the rotation speed influence coefficient is obtained by weighted calculation of the density of the reaction product, the temperature of the reaction product, the viscosity of the reaction product and the weight of the reaction product.

[0017] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0018] 1. The centrifugal filtration method for continuously preparing silane coupling agents in the present invention ensures that the olefins containing the catalyst and the hydrogen-containing silane can be fully and evenly mixed by using a mixing mechanism, thereby improving the reaction efficiency; the product after the reaction is centrifuged by the centrifugal mechanism, which can effectively separate the filtrate and remove impurities, thereby providing high-quality raw materials for subsequent distillation separation; and while the centrifugal treatment is being carried out, the mixing and reaction steps can be carried out simultaneously, thereby greatly improving the production efficiency.

[0019] 2. The mixing centrifugal device of the present invention integrates the mixing and centrifugal functions by providing a mixing mechanism and a centrifugal mechanism, thereby reducing the number of equipment required on the production line and saving production space. The close combination of the mixing and centrifugal functions enables the material to be continuously processed inside the mixing centrifugal device without the need for intermediate transfer, thereby saving energy consumption and time costs during transportation and improving production efficiency.

[0020] 3. The pipe adjusting assembly in the present invention is provided with a reciprocating screw, a movable seat and a connecting plate. When the discharge pipe is discharging material, the rotation of the reciprocating screw will cause the discharge pipe to move up and down reciprocatingly, thereby making the reaction products discharged from the discharge pipe more evenly distributed in the centrifuge barrel, avoiding accumulation and improving the separation effect.

[0021] 4. The driving assembly in the present invention is provided with a dual-axis motor, gears, reduction and transmission belt. The dual-axis motor drives the stirring assembly and the centrifugal assembly respectively through its upper and lower power output shafts, and can simultaneously complete the two major functions of mixing and centrifugation. This design can also reduce the number of driving sources required on the equipment, reducing the equipment manufacturing cost and maintenance cost.

[0022] 5. The centrifugal control system in the present invention integrates multiple modules such as data collection, analysis, and prediction, and can generate corresponding centrifugal speed levels according to the density, viscosity, temperature, and weight parameters of the reaction products, thereby ensuring the optimization of the centrifugal effect and effectively improving the separation efficiency and quality; the centrifugal control system can automatically adjust the centrifugal speed and duration according to the characteristics of the reaction products, which can avoid unnecessary energy waste and reduce energy consumption in the production process. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0024] Figure 1 This is a processing system diagram of the centrifugal filtration method for continuously preparing a silane coupling agent in the present invention;

[0025] Figure 2 The three-dimensional mixing centrifugal device of the present invention Figure 1 ;

[0026] Figure 3 The three-dimensional mixing centrifugal device of the present invention Figure 2 ;

[0027] Figure 4 It is a schematic diagram of the internal structure of the mixing cylinder and the fixed cylinder in the present invention;

[0028] Figure 5 It is a schematic diagram of the internal structure of the mixing cylinder in the present invention;

[0029] Figure 6 It is a schematic diagram of the internal structure of the centrifugal cylinder in the present invention;

[0030] Figure 7 It is a schematic diagram of the assembly structure of the centrifugal assembly and the driving assembly in the present invention;

[0031] Figure 8 It is a module diagram of the centrifugal control system in the present invention;

[0032] Figure numerals: 1, first material tank; 2, stirrer; 3, catalyst pipeline; 4, olefin pipeline; 5, first delivery pump; 6, first flow meter; 7, second material tank; 8, second delivery pump; 9, second flow meter; 10, mixing mechanism; 11, third delivery pump; 12, vacuum reaction distillation tower; 13, product storage tank; 20, centrifugal mechanism; 100, mixing cylinder; 101, connecting pipe; 102, first valve; 103, support column; 104, first delivery pipe; 105, second delivery pipe; 110, adding Shrink sleeve; 120, stirring assembly; 121, shaft; 122, stirring rod; 200, fixed cylinder; 201, discharge pipe; 202, second valve; 203, discharge pipe; 204, discharge pipe; 205, support leg; 210, centrifugal assembly; 211, centrifugal cylinder; 212, outer gear ring; 220, drive assembly; 221, dual-axis motor; 222, gear; 223, reducer; 224, transmission belt; 230, pipe adjustment assembly; 231, reciprocating screw; 232, moving seat; 233, connecting plate. DETAILED DESCRIPTION

[0033] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] Example 1

[0035] like Figure 1-Figure 4 As shown, the centrifugal filtration method for continuously preparing a silane coupling agent comprises the following steps:

[0036] Step 1, transporting the catalyst to the first material tank 1 through the catalyst pipeline 3, transporting the olefins to the first material tank 1 through the olefin pipeline 4, and then starting the agitator 2 to make the agitator 2 mix the catalyst and the olefins evenly to obtain the olefins containing the catalyst;

[0037] Step 2: transport the olefins containing the catalyst in the first material tank 1 to the mixing centrifugal device through the first delivery pump 5, and transport the hydrosilane in the second material tank 7 to the mixing centrifugal device through the second delivery pump 8, wherein a first flow meter 6 is installed on the delivery pipe of the first delivery pump 5, and a second flow meter 9 is installed on the delivery pipe of the second delivery pump 8;

[0038] Step 3: The mixing mechanism 10 in the mixing centrifugal device heats the olefins containing the catalyst and the hydrosilane to a reaction temperature of 10000 °C, and then stirs the olefins containing the catalyst and the hydrosilane to make the olefins containing the catalyst and the hydrosilane evenly mixed, and the olefins containing the catalyst and the hydrosilane react in the mixing mechanism 10 for 3 hours;

[0039] Step 4: After the reaction is completed, the first valve 102 is opened to allow the reaction product in the mixing mechanism 10 to enter the centrifugal mechanism 20 in the mixing centrifugal device, and steps 1 to 3 are repeated to allow new olefins containing catalyst and hydrosilane to react in the mixing mechanism 10;

[0040] Step 5: centrifuge the product after the reaction through the centrifuge mechanism 20 to obtain a filtrate;

[0041] Step 6: Start the third delivery pump 11 to extract the filtrate in the centrifugal mechanism 20 through the discharge pipe 203, and deliver the filtrate to the vacuum reaction distillation tower 12 for distillation separation to obtain a high-purity silane coupling agent;

[0042] Step 7: transport the high-purity silane coupling agent to the product storage tank 13 for storage.

[0043] In step 1, the olefin is selected from vinyl chloride and propylene chloride, and the catalyst is selected from chloroplatinic acid and its complex. In step 2, the hydrosilane is selected from trichlorosilane and dichlorodihydrosilane, and the molar ratio of the hydrosilane to the olefin is 1:1.5. In step 3, the reaction temperature can be 50 to 65 degrees Celsius.

[0044] The centrifugal filtration method for continuously preparing silane coupling agent ensures that the olefins containing the catalyst and the hydrogen-containing silane can be fully and evenly mixed by using a mixing mechanism 10, thereby improving the reaction efficiency; the centrifugal mechanism 20 is used to centrifuge the product after the reaction, so that the filtrate can be effectively separated and impurities can be removed, thereby providing high-quality raw materials for subsequent distillation separation; and the process flow is designed as a continuous production mode, that is, during the centrifugal treatment, the mixing and reaction steps can be carried out simultaneously, which greatly improves the production efficiency.

[0045] Example 2

[0046] like Figure 1-Figure 4 As shown, when other parts are the same as those of Example 1, the difference between this embodiment and Example 1 is that the mixing centrifugal device includes a mixing mechanism 10 and a centrifugal mechanism 20. The mixing mechanism 10 is used to heat and stir the olefins and hydrogen-containing silane containing the catalyst; the centrifugal mechanism 20 is located below the mixing mechanism 10, and the centrifugal mechanism 20 is used to receive the post-reaction product discharged from the mixing mechanism 10 and perform centrifugal treatment on the post-reaction product.

[0047] like Figure 4 and Figure 5 As shown, the mixing mechanism 10 includes a mixing barrel 100, a connecting pipe 101, a first valve 102, a first delivery pipe 104, a second delivery pipe 105, a heating jacket 110 and a stirring assembly 120. A plurality of support columns 103 are installed at the bottom of the mixing barrel 100, and the connecting pipe 101 is installed at the bottom of the mixing barrel 100, and the lower end of the connecting pipe 101 extends into the centrifugal mechanism 20. The first valve 102 is installed on the connecting pipe 101; the first delivery pipe 104 is installed on the side of the mixing barrel 100, and the other end of the first delivery pipe 104 is connected to the delivery pipe of the first delivery pump 5; the second delivery pipe 105 is installed on the side of the mixing barrel 100, and the other end of the second delivery pipe 105 is connected to the delivery pipe of the second delivery pump 8; the heating jacket 110 is sleeved on the mixing barrel 100, and the heating jacket 110 is used to heat the mixing barrel 100 and the materials in the mixing barrel 100; the stirring assembly 120 is used to stir the materials in the mixing barrel 100.

[0048] Specifically, when the first delivery pump 5 is in operation, it will deliver the olefins containing the catalyst to the first delivery pipe 104, and then deliver the olefins containing the catalyst to the mixing drum 100; when the second delivery pump 8 is in operation, it will deliver the hydrogen-containing silane to the second delivery pipe 105, and then deliver the hydrogen-containing silane to the mixing drum 100, and then start the heating sleeve 110 to heat the mixing drum 100, and then heat the olefins containing the catalyst and the hydrogen-containing silane in the mixing drum 100, so that the olefins containing the catalyst and the hydrogen-containing silane react in the mixing drum 100, and then stir the olefins containing the catalyst and the hydrogen-containing silane through the stirring component 120, so as to accelerate the reaction efficiency.

[0049] like Figure 5 As shown, the stirring assembly 120 includes a shaft 121 and a plurality of stirring rods 122. The shaft 121 penetrates the mixing barrel 100 and is rotatably connected to the mixing barrel 100; the plurality of stirring rods 122 are all located in the mixing barrel 100, and the plurality of stirring rods 122 are all fixedly connected to the shaft 121.

[0050] Specifically, when the shaft 121 rotates, the plurality of stirring rods 122 are driven to rotate, so that the plurality of stirring rods 122 stir the materials in the mixing barrel 100 to mix the materials evenly.

[0051] like Figure 4 , Figure 6 and Figure 7 As shown, the centrifugal mechanism 20 includes a fixed barrel 200, a discharge pipe 201, a second valve 202, a discharge pipe 203, a feed pipe 204, a centrifugal assembly 210 and a drive assembly 220. A plurality of support legs 205 are installed at the bottom of the fixed barrel 200. The fixed barrel 200 is installed directly below the mixing barrel 100. The lower ends of the plurality of support columns 103 are fixedly connected to the top surface of the fixed barrel 200. The lower end of the connecting pipe 101 passes through the top surface of the fixed barrel 200. The discharge pipe 201 is installed on the bottom surface of the fixed barrel 200. The second valve 202 is fixedly sleeved on the discharge pipe 201. The discharge pipe 203 is installed on the bottom surface of the fixed barrel 200 and is connected to the pumping pipe of the third delivery pump 11. The feed pipe 204 is slidably connected to the connecting pipe 101. The drive assembly 220 is used to drive the centrifugal assembly 210 to rotate.

[0052] Specifically, after the reaction of the olefins and hydrogen-containing silanes containing the catalyst in the mixing barrel 100 is completed, the second valve 202 is opened to allow the reaction product to enter the discharge pipe 204 through the discharge pipe 201 and then enter the centrifugal assembly 210. At the same time, the centrifugal assembly 210 is driven to rotate by the driving assembly 220, so that the reaction product is centrifuged, and the filtrate is separated outside the centrifugal assembly 210 and enters the discharge pipe 203.

[0053] like Figure 6 and Figure 7 As shown, the centrifugal assembly 210 includes a centrifugal cylinder 211 and an outer gear ring 212. The centrifugal cylinder 211 is rotatably mounted in the fixed cylinder 200, and the lower end of the connecting tube 101 is located in the centrifugal cylinder 211; the outer gear ring 212 is fixedly sleeved on the side of the centrifugal cylinder 211.

[0054] Specifically, the reaction products discharged through the connecting tube 101 will directly enter the centrifugal cylinder 211. When the outer gear ring 212 rotates, it will drive the centrifugal cylinder 211 to rotate, thereby facilitating the centrifugal treatment of the reaction products.

[0055] like Figure 6 and Figure 7 As shown, the driving assembly 220 includes a dual-axis motor 221, a gear 222, a reducer 223 and a transmission belt 224. The dual-axis motor 221 is mounted on the top surface of the fixed cylinder 200, and the lower power output shaft of the dual-axis motor 221 extends into the fixed cylinder 200 and is rotatably connected to the fixed cylinder 200; the gear 222 is mounted on the lower power output shaft of the dual-axis motor 221, and the gear 222 is meshed and connected with the outer gear ring 212; the reducer 223 is mounted on the mixing cylinder 100, and the input shaft of the reducer 223 is fixedly connected to the upper power output shaft of the dual-axis motor 221; the output shaft of the reducer 223 and the shaft 121 are fixedly sleeved with pulleys, and the transmission belt 224 is sleeved on the two pulleys.

[0056] Specifically, when the dual-axis motor 221 is running, the lower power output shaft of the dual-axis motor 221 will drive the gear 222 to rotate, and then engage and drive the outer gear ring 212 to rotate, and then drive the centrifuge barrel 211 to rotate; and when the dual-axis motor 221 is running, its upper power output shaft will start the reducer 223 to operate, and the output shaft of the reducer 223 will drive the shaft rod 121 to rotate through the transmission belt 224, and then drive the multiple stirring rods 122 to rotate.

[0057] like Figure 6 As shown, the centrifugal mechanism 20 also includes a pipe adjustment assembly 230, which includes a reciprocating screw 231, a moving seat 232 and a connecting plate 233. The reciprocating screw 231 penetrates the top surface of the fixed cylinder 200 and is rotatably connected to the fixed cylinder 200, and the upper end of the reciprocating screw 231 is fixedly connected to the lower end of the shaft 121; the moving seat 232 is sleeved on the reciprocating screw 231; the connecting plate 233 is fixedly sleeved on the moving seat 232, and the connecting plate 233 is fixedly connected to the feeding pipe 204.

[0058] Specifically, when the reciprocating screw 231 rotates, the moving seat 232 will move back and forth up and down along the reciprocating screw 231, thereby driving the connecting plate 233 to move back and forth up and down, and then driving the discharge pipe 204 to move back and forth up and down.

[0059] Working principle: When in use, the first delivery pump 5 is started to deliver the olefins containing the catalyst to the first delivery pipe 104, and then the olefins containing the catalyst are delivered to the mixing drum 100; the second delivery pump 8 is started to deliver the hydrogen-containing silane to the second delivery pipe 105, and then the hydrogen-containing silane is delivered to the mixing drum 100, and then the heating sleeve 110 is started to heat the mixing drum 100, and then the olefins containing the catalyst and the hydrogen-containing silane in the mixing drum 100 are heated, so that the olefins containing the catalyst and the hydrogen-containing silane react in the mixing drum 100.

[0060] At the same time, by starting the dual-axis motor 221, the upper power output shaft of the dual-axis motor 221 drives the reducer 223 to operate, and then the output shaft of the reducer 223 drives the shaft 121 to rotate through the transmission belt 224, and then drives the shaft 121 to rotate, and then drives the multiple stirring rods 122 to rotate, and then the multiple stirring rods 122 stir the olefins and hydrogen-containing silanes containing the catalyst, thereby accelerating the reaction efficiency.

[0061] After the olefins containing the catalyst and the hydrosilane react for 2-4 hours, the first valve 102 is opened to discharge the reaction product in the mixing drum 100 through the discharge pipe 201, and the reaction product in the discharge pipe 201 is discharged into the centrifugal drum 211 through the discharge pipe 204. Due to the operation of the dual-axis motor 221, the lower power output shaft of the dual-axis motor 221 drives the gear 222 to rotate, and then drives the outer gear ring 212 to rotate, and then drives the centrifugal drum 211 to rotate. The rotating centrifugal drum 211 centrifuges the reaction product, so that the filtrate is removed from the centrifugal drum 211.

[0062] When the dual-axis motor 221 is running, the shaft 121 will rotate, and the rotating shaft 121 will drive the reciprocating screw 231 to rotate, thereby causing the movable seat 232 to move back and forth up and down along the reciprocating screw 231, thereby driving the connecting plate 233 to move back and forth up and down, and then driving the discharge pipe 204 to move back and forth up and down, so that the post-reaction products discharged from the discharge pipe 204 are more evenly distributed in the centrifugal barrel 211, avoiding the accumulation of post-reaction products in a certain area of ​​the centrifugal barrel 211, thereby improving the separation effect.

[0063] After centrifugation is completed, the filtrate will enter the discharge pipe 203 to prepare for the next process, and the objects blocked by the centrifuge cylinder 211 will enter the discharge pipe 201.

[0064] Among them, when the reaction products in the fixed cylinder 200 enter the centrifugal cylinder 211 through the discharge pipe 201 and the down pipe 204, the olefins containing the catalyst and the hydrogen-containing silane can be transported to the mixing cylinder 100 by starting the first delivery pump 5 and the second delivery pump 8. Then, the olefins containing the catalyst and the hydrogen-containing silane are heated and stirred to make the olefins containing the catalyst and the hydrogen-containing silane react in the mixing cylinder 100, thereby facilitating the improvement of production efficiency.

[0065] Example 3

[0066] like Figure 2 , Figure 7 and Figure 8 As shown, when other parts are the same as those in Example 2, the difference between this embodiment and Example 2 is that the mixing centrifugal device also includes a centrifugal control system, and the mixing centrifugal device is used to control the centrifugal time.

[0067] The centrifugal control system includes a data collection module, a data analysis module, a data acquisition module and a time prediction module. The modules are connected by wired / wireless means to realize data transmission.

[0068] A data acquisition module, used to collect comprehensive data information of the mixing centrifugal device, wherein the comprehensive data information includes the density of the reaction product in the centrifugal cylinder 211, the temperature of the reaction product, the viscosity of the reaction product and the weight of the reaction product;

[0069] The data analysis module generates a speed influence coefficient according to the comprehensive data information, and generates a corresponding centrifugal speed level according to the speed influence coefficient;

[0070] The speed influence coefficient is generated as follows:

[0071]

[0072] Wherein, L is the speed influence coefficient, Md is the density of the product after the reaction, Dd is the viscosity of the product after the reaction, Wd is the temperature of the product after the reaction, Zl is the weight of the product after the reaction, and are all weight coefficients, which are determined by technicians in this field according to specific application requirements. and All are greater than 0;

[0073] Specifically, the greater the density of the product after the reaction, the greater the centrifugal force required, and the centrifugal speed also needs to be increased accordingly to overcome the larger inertial force and achieve effective separation. The density of the product after the reaction can be measured and obtained by a density sensor.

[0074] The higher the temperature of the reaction product, the lower the viscosity of the reaction product, the smaller the resistance between the solid particles and the liquid during the centrifugation process, and the easier the separation. The temperature of the reaction product is an important factor affecting the interaction forces between particles in the material (such as van der Waals forces, electrostatic forces, etc.). At high temperatures, these interaction forces will weaken, making the particles easier to disperse. On the contrary, at low temperatures, these forces will increase, causing particles to aggregate. Therefore, the higher the temperature of the reaction product, the weaker the interaction forces between the particles, the easier the particles are to disperse, and the easier the separation is. The temperature of the reaction product is measured by a temperature sensor.

[0075] The greater the viscosity of the reaction product, the greater the difficulty of solid-liquid separation during centrifugation, the greater the centrifugal force required, and the centrifugal speed also needs to be increased accordingly. The viscosity of the reaction product can be measured by a viscosity sensor. The greater the weight of the reaction product, in order to maintain the same centrifugal effect, a greater centrifugal force is required to separate it, and the speed needs to be increased to increase the centrifugal force. The weight of the reaction product is measured by a weight sensor, first by measuring the weight of the centrifuge cylinder 211 with the reaction product, and then subtracting the weight of the empty centrifuge cylinder 211 from the weight of the centrifuge cylinder 211 with the reaction product, that is, the weight of the reaction product located in the centrifuge cylinder 211 is obtained.

[0076] It should be noted that the formulas involved in the above-mentioned are all calculated by removing dimensions and taking numerical values. They are a formula that is closest to the actual situation obtained by collecting a large amount of data and performing software simulation. The weight coefficients in the formulas and the various preset thresholds in the analysis process are set by technical personnel in this field according to actual conditions or obtained by simulating a large amount of data; the size of the weight coefficient is to quantify each parameter to obtain a specific value for subsequent comparison. The size of the weight coefficient depends on the amount of sample data and the corresponding processing coefficients initially set by technical personnel in this field for each group of sample data; as long as it does not affect the proportional relationship between the parameters and the quantized values.

[0077] The centrifugal speed levels are generated as follows:

[0078] The centrifugal speed levels include primary speed, secondary speed and tertiary speed, wherein the primary speed, secondary speed and tertiary speed increase in sequence, and the primary speed, secondary speed and tertiary speed are all the speeds of the dual-axis motor 221. When the dual-axis motor 221 is running, it will drive the centrifugal cylinder 211 to rotate through the gear 222 and the outer gear ring 212. By adjusting the speed of the dual-axis motor 221, the rotation of the centrifugal cylinder 211 can be adjusted, thereby adjusting the centrifugal speed;

[0079] The threshold range of the preset speed influence coefficient is L1, L2, L1 <L2;

[0080] If L≤L1, at this time, the data analysis module generates a first-level speed;

[0081] If L2≥L>L1, at this time, the data analysis module generates a secondary speed;

[0082] If L>L2, at this time, the data analysis module generates three levels of speed.

[0083] Among them, L1 and L2 are determined by technical personnel in this field according to specific application requirements.

[0084] Exemplarily, the speeds of the dual-axis motor 221 corresponding to the first-level speed, the second-level speed, and the third-level speed are 5000 rpm, 8000 rpm, and 12000 rpm, respectively; the speed of the dual-axis motor 221 can also be customized according to specific circumstances; the speed of the dual-axis motor 221 is controlled according to the corresponding centrifugal speed level.

[0085] A data acquisition module is used to collect a historical training data set of the hybrid centrifugal device, the historical training data set includes speed comprehensive impact data and centrifugal duration; wherein the speed comprehensive impact data includes comprehensive data information and speed data of the dual-axis motor 221, and the speed data of the dual-axis motor 221 can be obtained through a Hall effect sensor;

[0086] The centrifugation time refers to the time required to centrifuge the reaction product in the centrifuge tube 211 , and the centrifugation time can be obtained by a timer.

[0087] The time prediction module trains a machine learning model for predicting centrifugal duration based on a historical training data set, collects comprehensive impact data of real-time rotation speed, and inputs it into the trained machine learning model to predict centrifugal duration;

[0088] The training method of the machine learning model for predicting centrifugal duration includes:

[0089] Convert the collected speed comprehensive influence data into a corresponding set of feature vectors;

[0090] Each set of feature vectors is used as the input of the machine learning model. The machine learning model takes the centrifugal time corresponding to each set of speed comprehensive impact data as the output, takes the centrifugal time actually corresponding to each set of speed comprehensive impact data as the prediction target, and takes minimizing the loss function value of the machine learning model as the training target; training is stopped when the loss function value of the machine learning model is less than or equal to the preset target loss value.

[0091] The machine learning model can be one of the models such as SVM regression, random forest regression or neural network regression.

[0092] The loss function value of the machine learning model is the mean square error;

[0093] Mean square error is one of the commonly used loss functions. Minimization is used as the goal to train the model so that the machine learning model better fits the data, thereby improving the performance and accuracy of the model;

[0094] In the loss function, MSE is the loss function value of the machine learning model, x is the feature vector group number; m is the number of feature vector groups; y is the number of feature vector groups; x is the centrifugal duration predicted by the x-th group of feature vectors, □ x is the actual centrifugal duration corresponding to the xth group of eigenvectors;

[0095] Other model parameters of the machine learning model, target loss value, optimization algorithm, training set test set validation set ratio, and loss function optimization are all achieved through actual engineering implementation and continuous experimental tuning.

[0096] The running time of the dual-axis motor 221 is controlled according to the predicted centrifugal duration; when the running time of the dual-axis motor 221 is the same as the predicted centrifugal duration, the dual-axis motor 221 is controlled to be powered off and stop running.

[0097] In summary, the centrifugal control system integrates multiple modules such as data acquisition, analysis, and prediction. It can generate corresponding centrifugal speed levels according to the density, viscosity, temperature, and weight parameters of the reaction products, thereby ensuring the optimization of the centrifugal effect and effectively improving the separation efficiency and quality. The centrifugal control system can automatically adjust the centrifugal speed and duration according to the characteristics of the reaction products, which can avoid unnecessary energy waste and reduce energy consumption in the production process.

[0098] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

[0099] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A centrifugal filtration method for continuously preparing a silane coupling agent, characterized in that: The steps include: Step 1: transporting the catalyst into the first material tank (1) through the catalyst pipeline (3), transporting the olefins into the first material tank (1) through the olefin pipeline (4), and mixing the two uniformly through the stirrer (2) to obtain olefins containing the catalyst; Step 2: transporting the olefins containing the catalyst in the first material tank (1) to the mixing centrifugal device via the first delivery pump (5), and transporting the hydrosilane in the second material tank (7) to the mixing centrifugal device via the second delivery pump (8); Step 3: The mixing mechanism (10) in the mixing centrifugal device heats the olefins containing the catalyst and the hydrosilane to a reaction temperature, and then stirs the olefins containing the catalyst and the hydrosilane to allow the olefins containing the catalyst and the hydrosilane to react in the mixing mechanism (10) for 2-4 hours; Step 4: transport the reaction product in the mixing mechanism (10) to the centrifugal mechanism (20) in the mixing centrifugal device; repeat steps 1 to 3 to allow new olefins containing the catalyst and the hydrosilane to react in the mixing mechanism (10); Step 5: centrifuging the product after the reaction through a centrifugal mechanism (20) to obtain a filtrate; Step 6: Start the third delivery pump (11) to extract the filtrate in the centrifugal mechanism (20), and deliver the filtrate to the vacuum reaction distillation tower (12) for distillation separation to obtain a high-purity silane coupling agent; Step 7: transport the high-purity silane coupling agent to the product storage tank (13) for storage.

2. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 1, characterized in that: The mixing centrifugal device comprises: A mixing mechanism (10) for heating and stirring the olefins and the hydrosilane containing the catalyst; The centrifugal mechanism (20) is located below the mixing mechanism (10) and is used to receive the post-reaction product discharged from the mixing mechanism (10) and perform centrifugal treatment on the post-reaction product.

3. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 2, characterized in that: The mixing mechanism (10) comprises: Mixing cylinder (100); A connecting pipe (101) installed at the bottom of the mixing cylinder (100); A first valve (102) installed on the connecting pipe (101); A first delivery pipe (104) is installed on the side of the mixing cylinder (100), and the other end of the first delivery pipe is connected to the delivery pipe of the first delivery pump (5); A second delivery pipe (105) is installed on the side of the mixing cylinder (100), and the other end of the second delivery pipe is connected to the delivery pipe of the second delivery pump (8); A heating sleeve (110), sleeved on the mixing barrel (100), and used for heating the material in the mixing barrel (100); The stirring assembly (120) is used to stir the material in the mixing barrel (100).

4. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 3, characterized in that: The stirring assembly (120) comprises: A shaft (121) passes through the mixing barrel (100) and is rotatably connected to the mixing barrel (100); A plurality of stirring rods (122) are located in the mixing barrel (100) and are fixedly connected to the shaft (121).

5. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 4, characterized in that: The centrifugal mechanism (20) comprises: The fixed cylinder (200) is installed directly below the mixing cylinder (100), and the lower end of the connecting pipe (101) penetrates the top surface of the fixed cylinder (200); A discharge pipe (201) is installed on the bottom surface of the fixed cylinder (200); A second valve (202) is fixedly sleeved on the discharge pipe (201); A liquid discharge pipe (203) is installed on the bottom surface of the fixed cylinder (200) and is connected to the extraction pipe of the third delivery pump (11); A feeding pipe (204) is slidably connected to the connecting pipe (101); Centrifugal assembly (210); The driving assembly (220) is used to drive the centrifugal assembly (210) to rotate.

6. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 5, characterized in that: The centrifugal assembly (210) comprises: A centrifugal cylinder (211) is rotatably mounted in the fixed cylinder (200), and the lower end of the connecting tube (101) is located in the centrifugal cylinder (211); The outer gear ring (212) is fixedly sleeved on the side of the centrifugal cylinder (211).

7. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 6, characterized in that: The driving assembly (220) comprises: A dual-axis motor (221) is mounted on the top surface of the fixed cylinder (200), and its lower power output shaft extends into the fixed cylinder (200) and is rotatably connected to the fixed cylinder (200); A gear (222) is mounted on the lower power output shaft of the dual-shaft motor (221) and is meshedly connected with the outer gear ring (212); A reducer (223) is mounted on the mixing drum (100), and its input shaft is fixedly connected to the upper power output shaft of the dual-shaft motor (221); A transmission belt (224) is sleeved on the output shaft of the reducer (223) and the shaft (121).

8. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 5, characterized in that: The centrifugal mechanism (20) further comprises a pipe adjustment assembly (230), wherein the pipe adjustment assembly (230) comprises: A reciprocating screw (231), which passes through the top surface of the fixed cylinder (200) and is rotatably connected to the fixed cylinder (200), and whose upper end is fixedly connected to the lower end of the shaft (121); A movable seat (232) sleeved on the reciprocating screw (231); The connecting plate (233) is fixedly sleeved on the movable seat (232) and fixedly connected to the feeding pipe (204).

9. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 7, characterized in that: The hybrid centrifugal device also includes a centrifugal control system, which includes: A data collection module, used for collecting comprehensive data information of the mixing centrifugal device, wherein the comprehensive data information includes the density of the reaction product in the centrifugal cylinder (211), the temperature of the reaction product, the viscosity of the reaction product and the weight of the reaction product; The data analysis module generates a speed influence coefficient according to the comprehensive data information, and generates a corresponding centrifugal speed level according to the speed influence coefficient; A data acquisition module is used to collect a historical training data set of the hybrid centrifugal device, the historical training data set including speed comprehensive impact data and centrifugal duration; the speed comprehensive impact data includes comprehensive data information and speed data of the dual-axis motor (221); The time prediction module trains a machine learning model for predicting centrifugal duration based on a historical training data set, collects comprehensive impact data of real-time rotation speed, and inputs it into the trained machine learning model to predict the centrifugal duration.

10. The centrifugal filtration method for continuously preparing a silane coupling agent according to claim 9, characterized in that: The rotation speed influence coefficient is obtained by weighted calculation of the density of the product after the reaction, the temperature of the product after the reaction, the viscosity of the product after the reaction and the weight of the product after the reaction.

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