A kind of production device and production method of silane coupling agent

Abstract

The present invention relates to the technical field of silane coupling agent production, and in particular to a silane coupling agent production device and a production method thereof. The production device includes a reaction kettle and a separation device connected in sequence, the separation device includes a rectangular shell, a drainage area is provided on one side of the shell, and a feed area and an activated carbon area are provided on the other side from top to bottom, a water-permeable plate is provided between the drainage area and the feed area, a first baffle is provided between the drainage area and the activated carbon area, a second baffle is provided between the feed area and the activated carbon area, the second baffle is provided with a plurality of through holes, a second filter plate is provided above, the second filter plate is connected to a lifting drive mechanism, and a sealing plug for blocking the through holes is provided on the lower end surface. The production device in the present invention has a compact structure, a small number of equipment, a small footprint, and high production efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of silane coupling agent production, and in particular to a silane coupling agent production device and a production method thereof. Background Art

[0002] The chemical name of silane coupling agent Si-69 is bis-[γ-(triethoxysilyl)propyl] tetrasulfide, which is often used to treat carbon black, SiO2 and other inorganic fillers. It not only has the functions of activator and coupling agent, but also has the functions of cross-linking agent, softener and reinforcing agent. It is used as reinforcing agent and vulcanizing agent in rubber industry. The synthesis method of Si-69 is: it is obtained by reacting γ-chloropropyltriethoxysilane with disodium tetrasulfide, and disodium tetrasulfide is obtained by reacting sodium hydroxide solution with sulfur.

[0003] The patent with application number 202110257002.9 discloses a device and method for optimizing the production of silane coupling agents. The production device includes a stirring synthesis chamber, a feed hopper, a No. 1 motor, a cooling and standing chamber, a filter chamber, an alkali liquid tank, and a blower; a mixing and stirring shaft and a suspended nozzle are arranged in the stirring and synthesis chamber, and a burette connected to the stirring and synthesis chamber is rotationally connected to the mixing and stirring shaft; an extrusion roller for grinding raw materials is arranged in the feed hopper, a guide pipe and a semipermeable membrane for separating the water layer and the organic layer are arranged in the standing cooling chamber, and the filter chamber is used for filtering and sending the filtrate to the purification device for distillation and purification. The production method is: raw material preparation, feeding, synthesis reaction, standing separation, filtration, and purification. This technical solution stirs and mixes while adding raw materials, which shortens the time of crude product synthesis reaction and improves production efficiency, but there are the following problems:

[0004] 1. In the stage of synthesizing crude products, the mixing and stirring efficiency can be improved by changing the mixing and stirring methods, but the reaction time cannot be significantly shortened. The subsequent process time of dehydration, filtration and decolorization of the crude products leads to limited improvement in production efficiency in the entire production process;

[0005] 2. When the crude product is subjected to preliminary separation and purification such as dehydration, filtration and decolorization, multiple sets of equipment are required, which has many processes, a large equipment footprint and low production efficiency;

[0006] 3. During the dehydration process, the semipermeable membrane used to separate the water layer and the organic layer is set horizontally. The solid impurities in the crude product will be deposited on the surface of the semipermeable membrane under the action of gravity, affecting the dehydration efficiency and service life of the semipermeable membrane;

[0007] In summary, there is an urgent need to provide a production device for a silane coupling agent with a compact structure, a small number of equipment, a small footprint, and high production efficiency. Summary of the invention

[0008] In order to solve at least one of the above technical problems, the present invention provides a production device of a silane coupling agent, comprising a reaction kettle and a separation device connected in sequence, the separation device comprising a rectangular shell, a drainage area is provided on one side of the shell, and a feed area and an activated carbon area are provided on the other side from top to bottom, a water-permeable plate is provided between the drainage area and the feed area, a first baffle is provided between the drainage area and the activated carbon area, a second baffle is provided between the feed area and the activated carbon area, the second baffle is provided with a plurality of through holes, a second filter plate is provided on the top, the second filter plate is connected to a lifting drive mechanism, and a sealing plug for blocking the through holes is provided on the lower end surface.

[0009] Preferably, a feed port is provided at the top of the feed zone, a scraper is provided circumferentially of the second filter plate to abut the side wall of the feed zone, the upper end surface of the second baffle is flush with the upper end surface of the first baffle, a limit block supporting the second baffle is provided above the side wall of the activated carbon zone, a discharge port and an activated carbon filling port are provided below the side wall, a sealing cover is provided on the activated carbon filling port, a filter screen and a first electric valve are provided on the discharge port, and a water outlet is provided at the bottom of the drainage zone.

[0010] Preferably, the water-permeable plate includes a first filter plate facing the feed area and a water-permeable membrane facing the drainage area, the water-permeable plate is detachably mounted on the upper end surface of the first baffle, the first baffle is fixed to the bottom of the shell, the shell includes a shell body with an open top, an upper cover is provided on the top of the shell body, and legs are provided on the bottom, the activated carbon area is provided with a stirring paddle, and the bottom of the shell is provided with a motor connected to the stirring paddle.

[0011] Preferably, the sealing plug comprises a thin cylindrical section connected to the second filter plate, the bottom of the thin cylindrical section is connected to a conical section whose diameter increases downward, the bottom of the conical section is connected to a thick cylindrical section, and the thick cylindrical section blocks the through hole.

[0012] Preferably, the upper end surface of the second baffle is provided with an "inverted L"-shaped first hook, and the lower end surface of the second filter plate is provided with an "L"-shaped second hook, and the first hook and the second hook are slidably engaged in the vertical direction.

[0013] Preferably, the lifting drive mechanism includes a liquid storage cylinder, which is connected to a vertically arranged hydraulic telescopic sleeve, and the hydraulic telescopic sleeve is connected to the second filter plate; the liquid storage cylinder includes a closed cylinder body, and a piston is provided inside the cylinder body, and the piston seals and separates the cylinder body into a first hydraulic chamber and a second hydraulic chamber, the first hydraulic chamber is provided with a liquid inlet, and the second hydraulic chamber is connected to the hydraulic telescopic sleeve.

[0014] Preferably, the cylinder body and the piston are both annular, the cylinder body is arranged at the bottom of the shell, the liquid inlet is arranged below the side wall of the cylinder body, the piston is arranged above the liquid inlet, and a support rod is arranged at the bottom.

[0015] Preferably, the hydraulic telescopic sleeve includes a fixed cylinder that is sealed and passes through the shell, an intermediate slide cylinder is sealingly and slidingly sleeved inside the fixed cylinder, a piston rod is slidingly provided inside the intermediate slide cylinder, the fixed cylinder is fixed on the cylinder body and is sealed and connected with the second hydraulic chamber, the intermediate slide cylinder includes a plurality of cylinders that are sealingly and slidingly sleeved, and the piston rod can pass through the through hole and be connected to the sealing plug.

[0016] Preferably, an overflow port is provided on the side wall of the drainage area, the upper end surface of the overflow port is flush with the upper end surface of the first baffle, a connecting pipe connects the water outlet and the liquid inlet, a second electric valve is provided on the connecting pipe, a drain port is provided at the bottom of the cylinder body, and a third electric valve is provided on the drain port.

[0017] The present invention provides a method for producing a silane coupling agent, which is produced by using the above-mentioned silane coupling agent production device, and comprises the following steps:

[0018] Step S100, adding measured sodium hydroxide, sulfur and deionized water into a reaction kettle, stirring and heating to 50-70° C., and continuing the reaction for 15-30 minutes after the solid is completely dissolved;

[0019] Step S200, raising the temperature of the reaction kettle to 75-85° C., adding a measured amount of γ-chloropropyltriethoxysilane dropwise into the reaction kettle, and continuing the reaction for 20-30 minutes after the addition is complete to obtain a crude product of silane coupling agent Si-69;

[0020] Step S300, cooling the crude product in the reactor to below 40°C, and then passing the crude product into the feed area of ​​the separation device, and the water in the crude product enters the drainage area through the permeable plate for dehydration;

[0021] Step S400, after dehydration is completed, the lifting drive mechanism drives the second filter plate to slowly rise to the top of the shell, and the solid impurities in the dehydrated crude product are trapped on the upper surface of the second filter plate;

[0022] Step S500, while the second filter plate rises, the sealing plug is separated from the through hole of the second baffle plate, and the crude product after dehydration and filtration enters the activated carbon area from the through hole, and the activated carbon in the activated carbon area decolorizes the crude product after dehydration and filtration, and a purified product is obtained after the decolorization is completed;

[0023] Step S600, passing the purified product into a distillation kettle, and obtaining the silane coupling agent Si-69 after negative pressure distillation.

[0024] Compared with the prior art, the present invention has the following beneficial technical effects:

[0025] 1. The present invention synthesizes a crude product of silane coupling agent Si-69 through a reaction kettle, and then passes the crude product into a separation device for dehydration, filtration and decolorization. The number of equipment is small, the material conversion and transportation between each process is reduced, and the production efficiency is improved;

[0026] 2. The water-permeable plate in the separation device adopts a non-traditional vertical setting, which is not easily blocked by solid impurities during the dehydration process and has a longer service life; the water-permeable plate is composed of a first filter plate and a water-permeable membrane. The first filter plate can filter solid impurities in the crude product and form a protective layer for the water-permeable membrane, which can not only further extend the service life of the water-permeable membrane, but also improve the structural strength of the water-permeable plate;

[0027] 3. The feed area and activated carbon area of ​​the separation device can be connected or closed with the lifting and lowering of the second filter plate, so that the filtering and impurity removal of the dehydrated crude product and the decolorization process can be carried out simultaneously, which improves the production efficiency; the scraper on the second filter plate can clean the water-permeable plate and the inner wall of the shell during the lifting process, avoid clogging of the water-permeable plate and keep the inner wall of the shell clean. When the second filter plate rises to the top of the shell, the feed chamber is substantially converted into a decolorization chamber as a whole. The dynamic conversion of the feed chamber and the decolorization chamber can make full use of the internal space of the shell, making the overall structure of the equipment compact and greatly reducing the volume of the equipment;

[0028] 4. The first baffle, the second baffle, the shell and the sealing plug together enclose a closed activated carbon area. When the crude product is dehydrated in the feed area, it cannot enter the closed activated carbon area, thereby improving the service life and decolorization effect of the activated carbon;

[0029] 5. The sealing plug at the bottom of the second filter plate is connected to the second filter plate through a thin cylindrical section, which can reduce the obstruction of the second filter plate and ensure that the filtering area of ​​the second filter plate is not affected. The thick cylindrical section blocks the through hole, which is convenient for increasing the diameter of the through hole on the second baffle plate and improving the rate at which the coarse product after dehydration and filtration passes through the second baffle plate. The use of a conical section to connect the thin cylindrical section and the thick cylindrical section can reduce the rising resistance of the second filter plate;

[0030] 6. The second baffle plate and the second filter plate are dynamically connected by the first hook and the second hook, so that the distance between the second baffle plate and the second filter plate can be changed within a certain range, so as to ensure that the sealing plug can be inserted into or removed from the through hole, so that the activated carbon area becomes an open area with an opening at the top under control, which greatly improves the decolorization efficiency;

[0031] 7. The lifting drive mechanism adopts a structure in which a liquid storage cylinder and a hydraulic telescopic sleeve are used together. On the premise of meeting the lifting distance of the second filter plate, the height of the liquid storage cylinder can be greatly reduced, making the equipment more compact;

[0032] 8. Directly use the water in the drainage area as the pressure liquid and inject it into the liquid storage cylinder to control the extension and retraction of the hydraulic telescopic sleeve. No additional pressure liquid injection equipment is required, which reduces production costs;

[0033] In summary, the production device of the present invention has a compact structure, a small number of equipment, a small footprint and high production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a structural schematic diagram of the present invention;

[0035] Figure 2 is a three-dimensional cross-sectional view of the separation device;

[0036] Figure 3 is a schematic structural diagram of the second baffle;

[0037] Figure 4 is a schematic diagram of the structure of the second filter plate;

[0038] Figure 5 is a three-dimensional cross-sectional view of a liquid storage cylinder;

[0039] Figure 6 It is a three-dimensional cross-sectional view of a hydraulic telescopic sleeve;

[0040] Figure 7 It is a front view of the separation device in Example 1;

[0041] Figure 8 It is a structural schematic diagram of the separation device in the decolorization state;

[0042] Fig. 9 This is the front view of the separation device in Example 2.

[0043] 1. Reactor, 2. Separation device, 21. Shell, 211. Shell body, 2111. Limit block, 2112. Discharge port, 2113. Filter, 2114. First electric valve, 2115. Water outlet, 2116. Activated carbon filling port, 2117. Sealing cover, 2118. Overflow port, 212. Upper cover, 2121. Feed port, 213. Legs, 22. Permeable plate, 221. First filter plate, 222. Permeable membrane, 23. First baffle, 24. Second baffle, 241. Through hole, 242. First hook, 25. Second filter plate, 251. Sealing plug, 252. Second hook, 2511. Thin round Column section, 2512, conical section, 2513, thick cylindrical section, 253, scraper, 26, lifting drive mechanism, 261, liquid storage cylinder, 2611, cylinder body, 2612, piston, 2613, first hydraulic chamber, 2614, second hydraulic chamber, 2615, liquid inlet, 2616, support rod, 2617, liquid discharge port, 2618, third electric valve, 262, hydraulic telescopic sleeve, 2621, fixed cylinder, 2622, middle sliding cylinder, 2623, piston rod, 27, stirring paddle, 28, motor, 29, connecting pipe, 291, second electric valve, 10, feeding area, 20, activated carbon area, 30, drainage area. DETAILED DESCRIPTION

[0044] The specific implementation of the present invention is described below in conjunction with the accompanying drawings and embodiments:

[0045] It should be noted that the structures, proportions, sizes, etc. illustrated in the drawings of this specification are only used to match the contents disclosed in the specification so that people familiar with this technology can understand and read them, and are not used to limit the conditions under which the present invention can be implemented. Any structural modification, change in proportional relationship or adjustment of size should fall within the scope of the technical contents disclosed in the present invention without affecting the effects and purposes that can be achieved by the present invention.

[0046] At the same time, the terms such as "upper", "lower", "left", "right", "middle" and "one" cited in this specification are only for the convenience of description and are not used to limit the scope of implementation of the present invention. Changes or adjustments to their relative relationships should be regarded as the scope of implementation of the present invention without substantially changing the technical content. Example 1

[0047] Combined with Figure 1-8The present embodiment provides a production device of a silane coupling agent, comprising a reaction kettle 1 and a separation device 2 connected in sequence, wherein the separation device 2 comprises a rectangular shell 21, wherein a drainage area 30 is provided on one side of the shell 21, and a feed area 10 and an activated carbon area 20 are provided on the other side from top to bottom, respectively, a water permeable plate 22 is provided between the drainage area 30 and the feed area 10, and a first baffle 23 is provided between the drainage area 30 and the activated carbon area 20, a second baffle 24 is provided between the feed area 10 and the activated carbon area 20, the second baffle 24 is provided with a plurality of through holes 241, a second filter plate 25 is provided on the upper side, the second filter plate 25 is connected to a lifting drive mechanism 26, and a sealing plug 251 for blocking the through holes 241 is provided on the lower end surface.

[0048] In the above technical scheme, the water-permeable plate 22 refers to a partition containing a high molecular polymer for separating water and organic matter, which can allow water in the crude product of silane coupling agent to pass through and dehydrate the crude product of silane coupling agent. The water-permeable plate 22 in the present invention is a vertical plate rather than a traditional horizontal plate. During the dehydration process, solid impurities in the crude product fall vertically under the action of gravity and are not easily deposited on the water-permeable plate 22, which can avoid clogging of the water-permeable plate 22 and extend its service life; the lifting drive mechanism 26 can directly adopt conventional lifting drive equipment such as cylinders or hydraulic cylinders, which can drive the second filter plate 25 to rise and fall; during production, the reaction raw materials react in the reactor 1 to obtain the crude product of silane coupling agent, and the crude product is passed into the feed area 10 of the separation device 2 for dehydration, and the water in the crude product passes through the water-permeable plate 22 into the drainage area 30 on one side. After dehydration, the feed The remaining dehydrated crude product in the zone 10 is driven to rise by the second filter plate 25 through the lifting drive mechanism 26. The second filter plate 25 rises above the liquid level of the dehydrated crude product and stops after reaching the top of the feed zone 10. The second filter plate 25 filters the dehydrated crude product during the rising process, and retains solid impurities on the upper end surface of the second filter plate 25. The crude product after dehydration and filtration is below the second filter plate 25. During the rising process of the second filter plate 25, the sealing plug 251 on the lower end surface of the second filter plate 25 is separated from the through hole 241 of the second baffle 24, and the crude product after dehydration and filtration enters the activated carbon zone 20 from the through hole 241. The crude product after dehydration and filtration is decolorized in the activated carbon zone 20. After the decolorization is completed, the purified product of the silane coupling agent is obtained. The purified product is passed into a distillation kettle for distillation and refining. After removing trace moisture and impurities, the finished silane coupling agent can be obtained.

[0049] In the prior art, when purifying the crude product, it is necessary to sequentially equip multiple sets of equipment such as dehydration, filtration and decolorization, which has many processes, large equipment footprint and low production efficiency. The separation device 2 in this embodiment only needs one set of equipment to achieve dehydration, filtration and decolorization of the crude silane coupling agent product, and the number of equipment used is small, eliminating the material conversion and transportation between the equipment, thereby improving production efficiency; the permeable plate 22 in the separation device 2 adopts a non-traditional vertical setting, which is not easily blocked by solid impurities during the dehydration process, and the service life is extended; the feed zone 10 and the activated carbon zone 20 of the separation device 2 can be connected or closed with the rise and fall of the second filter plate 25, so that the filtration and impurity removal and decolorization processes of the dehydrated crude product can be carried out simultaneously, thereby improving production efficiency; when the second filter plate 25 rises to the top of the shell 21, the feed zone 10 is substantially converted into a decolorization chamber as a whole, and the dynamic conversion of the feed zone 10 and the decolorization chamber can make full use of the internal space of the shell 21, making the overall structure of the equipment compact and greatly reducing the volume of the equipment.

[0050] In a specific technical scheme, a feed port 2121 is provided at the top of the feed zone 10, a scraper 253 is circumferentially provided on the second filter plate 25 to abut against the side wall of the feed zone 10, the upper end surface of the second baffle 24 is flush with the upper end surface of the first baffle 23, a limit block 2111 is provided above the side wall of the activated carbon zone 20 to support the second baffle 24, a discharge port 2112 and an activated carbon filling port 2116 are provided below the side wall, a sealing cover 2117 is provided on the activated carbon filling port 2116, a filter screen 2113 and a first electric valve 2114 are provided on the discharge port 2112, and a water outlet 2115 is provided at the bottom of the drainage zone 30.

[0051] In the above technical solution, the scraper 253 can clean the water-permeable plate 22 and the inner wall of the shell 21 during the lifting and lowering of the second filter plate 25, further avoiding clogging of the water-permeable plate 22 and keeping the inner wall of the shell 21 clean. The upper end surface of the second baffle 24 is flush with the upper end surface of the first baffle 23, so that the first baffle 23, the second baffle 24, the shell 21 and the sealing plug 251 can be together to form a closed activated carbon area 20. When the crude product is dehydrated in the feed area 10, it cannot enter the closed activated carbon area 20, thereby improving the service life and decolorization effect of the activated carbon; in addition, the feed port 2121 is closed, and during the rising process of the second filter plate 25, the second filter plate 25 will produce a filter pressing effect on the dehydrated crude product above it, which can further improve the filtration efficiency.

[0052] In a specific technical solution, the water-permeable plate 22 includes a first filter plate 221 facing the feed area 10 and a water-permeable membrane 222 facing the drainage area 30. The water-permeable plate 22 is detachably mounted on the upper end surface of the first baffle 23. The first baffle 23 is fixed to the bottom of the shell 21. The shell 21 includes a shell body 211 with an open top. The top of the shell body 211 is provided with an upper cover 212 and the bottom is provided with support legs 213. The activated carbon area 20 is provided with a stirring paddle 27, and the bottom of the shell 21 is provided with a motor 28 connected to the stirring paddle 27.

[0053] In the above technical scheme, the first filter plate 221 can filter solid impurities in the crude product, form a protective layer for the water-permeable membrane 222, extend the service life of the water-permeable membrane 222, and improve the structural strength of the water-permeable plate 22; the water-permeable membrane 222 is a polymer separation membrane, which can allow water in the crude product to pass through; an upper cover 212 is arranged on the top of the shell 21, and after the production is completed, the upper cover can be opened to clean or replace the second filter plate 25 moved to the top of the shell 21; a stirring paddle 27 is arranged in the activated carbon zone 20 for stirring during decolorization, which can improve the decolorization efficiency.

[0054] In a specific technical solution, the sealing plug 251 includes a thin cylindrical section 2511 connected to the second filter plate 25, the bottom of the thin cylindrical section 2511 is connected to a conical section 2512 whose diameter increases downward, the bottom of the conical section 2512 is connected to a thick cylindrical section 2513, and the thick cylindrical section 2513 blocks the through hole 241.

[0055] In the above technical solution, the sealing plug 251 is connected to the second filter plate 25 through the thin cylindrical section 2511, which can reduce the obstruction of the second filter plate 25 and ensure that the filtering area of ​​the second filter plate 25 is not affected. The coarse cylindrical section 2513 blocks the through hole 241, which is convenient for increasing the diameter of the through hole 241 and improving the rate at which the coarse product after dehydration and filtration passes through the second baffle 24. The conical section 2512 is used to connect the thin cylindrical section 2511 and the coarse cylindrical section 2513, which can reduce the rising resistance of the second filter plate 25.

[0056] In a specific technical solution, the upper end surface of the second baffle 24 is provided with an "inverted L"-shaped first hook 242, and the lower end surface of the second filter plate 25 is provided with an "L"-shaped second hook 252, and the first hook 242 and the second hook 252 are slidably engaged in the vertical direction.

[0057] In the above technical solution, the second baffle plate 24 and the second filter plate 25 are dynamically connected by the first hook 242 and the second hook 252, so that the distance between the second baffle plate 24 and the second filter plate 25 is variable within a certain range, so as to ensure that the sealing plug 251 can be inserted into or out of the through hole 241. For example, in the initial state, the first hook 242 abuts against the lower end surface of the second filter plate 25, and the second hook 252 abuts against the upper end surface of the second baffle plate 24, and the distance between the second baffle plate 24 and the second filter plate 25 is the smallest. At this time, the sealing plug 251 of the second filter plate 25 blocks the second baffle plate 24. 24; when the lifting drive mechanism 26 drives the second filter plate 25 to move upward, the first hook 242 and the second hook 252 slide relative to each other. When the horizontal short sides of the first hook 242 and the second hook 252 are abutted and stuck, the distance between the second baffle plate 24 and the second filter plate 25 is the largest. At this time, the second filter plate 25 continues to rise, which will drive the second baffle plate 24 to rise until the second filter plate 25 and the second baffle plate 24 are both separated from the liquid surface of the dehydrated crude product. At this time, the activated carbon area 20 becomes an open area with an opening at the top, which greatly improves the decolorization efficiency.

[0058] In a specific technical solution, the lifting drive mechanism 26 includes a liquid storage cylinder 261, which is connected to a vertically arranged hydraulic telescopic sleeve 262, and the hydraulic telescopic sleeve 262 is connected to the second filter plate 25; the liquid storage cylinder 261 includes a closed cylinder body 2611, and a piston 2612 is provided inside the cylinder body 2611. The piston 2612 seals and separates the cylinder body 2611 into a first hydraulic chamber 2613 and a second hydraulic chamber 2614, and the first hydraulic chamber 2613 is provided with a liquid inlet 2615, and the second hydraulic chamber 2614 is connected to the hydraulic telescopic sleeve 262.

[0059] In the above technical scheme, the second hydraulic chamber 2614 is pre-loaded with pressure liquid, and the pressure liquid is introduced into or extracted from the first hydraulic chamber 2613 through the liquid inlet 2615, and the piston 2612 is controlled to move in a direction close to or away from the hydraulic telescopic sleeve 262, thereby changing the volume of the second hydraulic chamber 2614, so that the pressure liquid in the second hydraulic chamber 2614 flows into or out of the hydraulic telescopic sleeve 262, thereby controlling the extension or shortening of the hydraulic telescopic sleeve 262. The liquid storage cylinder 261 can be set at the top of the shell 21 or at the bottom of the shell 21. The liquid storage cylinder 261 and the hydraulic telescopic sleeve 262 are used in combination, which can greatly reduce the height of the liquid storage cylinder 261 while meeting the lifting distance of the second filter plate 25, making the equipment more compact.

[0060] In a specific technical solution, the cylinder body 2611 and the piston 2612 are both annular in shape, the cylinder body 2611 is arranged at the bottom of the shell 21, the liquid inlet 2615 is arranged below the side wall of the cylinder body 2611, the piston 2612 is arranged above the liquid inlet 2615, and a support rod 2616 is provided at the bottom.

[0061] In a specific technical solution, the hydraulic telescopic sleeve 262 includes a fixed cylinder 2621 that is sealed and passes through the shell 21, an intermediate slide cylinder 2622 is sealed and slidably sleeved inside the fixed cylinder 2621, a piston rod 2623 is slidably provided inside the intermediate slide cylinder 2622, the fixed cylinder 2621 is fixed on the cylinder body 2611 and is sealed and connected with the second hydraulic chamber 2614, the intermediate slide cylinder 2622 includes a plurality of sealed and slidably sleeved cylinders, and the piston rod 2623 can pass through the through hole 241 and be connected to the sealing plug 251.

[0062] In the above technical solution, the middle slide cylinder 2622 is composed of a plurality of sleeved and relatively sealable cylinders, which is a common structural design in the art. Figure 6 As shown, the cylinder in this embodiment has a circular sealing sliding flange on the bottom outer wall, a circular sealing limiting flange on the top inner wall, a circular sealing limiting flange on the top inner wall of the fixed cylinder 2621, and a circular sealing sliding flange on the bottom outer wall of the piston rod 2623; the piston rod 2623 is directly connected to the sealing plug 251, which can reduce the number of openings on the second filter plate 25 and reduce the shielding area of ​​the second filter plate 25, as shown in FIG. Figure 8 As shown, when two hydraulic telescopic sleeves 262 are equidistantly arranged on the circumference, the through holes 241 on the second baffle plate 24 and the sealing plugs 251 on the second filter plate 25 can be arranged in an even number at corresponding equidistant intervals on the circumference, and then the piston rods 2623 of the two hydraulic telescopic sleeves 262 are connected to the lower end surfaces of two of the sealing plugs 251. Example 2

[0063] Combined with Fig. 9 This embodiment provides a production device for a silane coupling agent. On the basis of Embodiment 1, the water in the drainage area 30 is directly used as the pressure liquid, which is injected into the liquid storage cylinder 261 to control the extension and contraction of the hydraulic telescopic sleeve 262. No additional pressure liquid injection equipment is required, which reduces the production cost. It is particularly suitable for the case where the rising resistance of the second baffle 24 and the second filter plate 25 is small. The specific technical solution is as follows:

[0064] An overflow port 2118 is provided on the side wall of the drainage area 30, and the upper end surface of the overflow port 2118 is flush with the upper end surface of the first baffle 23. The connecting pipe 29 connects the water outlet 2115 and the liquid inlet 2615. A second electric valve 291 is provided on the connecting pipe 29. A drain port 2617 is provided at the bottom of the cylinder body 2611, and a third electric valve 2618 is provided on the drain port 2617.

[0065] In the above technical solution, an overflow port 2118 is provided on the side wall of the drainage area 30 so that the liquid level in the drainage area 30 is always maintained below the feed area 10, which can ensure that the crude product in the feed area 10 can be fully dehydrated. When the dehydration is completed, the second electric valve 291 is opened, and the water in the drainage area 30 enters the first hydraulic chamber 2613 of the cylinder body 2611 from the connecting pipe 29, the piston 2612 moves upward, and the pressure liquid in the second hydraulic chamber 2614 enters the hydraulic telescopic sleeve 262, the hydraulic telescopic sleeve 262 extends, and pushes the second filter plate 25 to move upward; when the production is completed, the third electric valve 2618 is opened, the water in the first hydraulic chamber 2613 flows out, the piston 2612 moves downward and resets, the volume of the second hydraulic chamber 2614 increases, and the pressure liquid in the hydraulic telescopic sleeve 262 flows back to the second hydraulic chamber 2614, the hydraulic telescopic sleeve 262 contracts, and drives the second filter plate 25 to reset. Example 3

[0066] This embodiment provides a method for producing a silane coupling agent, comprising the following steps:

[0067] Step S100, adding measured sodium hydroxide, sulfur and deionized water into the reaction kettle 1, stirring and heating to 50-70° C., and continuing the reaction for 15-30 minutes after the solid is completely dissolved;

[0068] Step S200, heating the reactor 1 to 75-85° C., adding a measured amount of γ-chloropropyltriethoxysilane dropwise into the reactor 1, and continuing the reaction for 20-30 minutes after the addition is complete to obtain a crude product of silane coupling agent Si-69;

[0069] Step S300, cooling the crude product in the reactor 1 to below 40°C, and then passing the crude product into the feed area 10 of the separation device 2, and the water in the crude product enters the drainage area 30 through the water-permeable plate 22 for dehydration;

[0070] Step S400, after dehydration is completed, the lifting drive mechanism 26 drives the second filter plate 25 to slowly rise to the top of the housing 21, and the solid impurities in the dehydrated crude product are trapped on the upper end surface of the second filter plate 25;

[0071] Step S500, while the second filter plate 25 rises, the sealing plug 251 is separated from the through hole 241 of the second baffle plate 24, and the crude product after dehydration and filtration enters the activated carbon area 20 from the through hole 241, and the activated carbon in the activated carbon area 20 decolorizes the crude product after dehydration and filtration, and a purified product is obtained after the decolorization is completed;

[0072] Step S600, passing the purified product into a distillation kettle, and obtaining the silane coupling agent Si-69 after negative pressure distillation.

[0073] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention shall be equivalent replacement modes and shall be included in the protection scope of the present invention.

Claims

1. A silane coupling agent production device, comprising a reaction kettle (1) and a separation device (2) connected in sequence, characterized in that: The separation device (2) comprises a rectangular shell (21), wherein a drainage area (30) is provided on one side of the shell (21), and a feed area (10) and an activated carbon area (20) are provided on the other side from top to bottom, respectively; a water permeable plate (22) is provided between the drainage area (30) and the feed area (10), and a first baffle (23) is provided between the drainage area (30) and the activated carbon area (20); a second baffle (24) is provided between the feed area (10) and the activated carbon area (20), and the second baffle (24) is provided with a plurality of through holes (241), and a second filter plate is provided above the second baffle (24). (25), the second filter plate (25) is connected to the lifting drive mechanism (26), and the lower end surface of the second filter plate (25) is provided with a sealing plug (251) for sealing the through hole (241). When the second filter plate (25) rises, the sealing plug (251) is separated from the through hole (241) of the second baffle plate (24), and the crude product after dehydration and filtration enters the activated carbon area (20) through the through hole (241); the water-permeable plate (22) includes a first filter plate (221) facing the feed area (10) and a water-permeable membrane (222) facing the drainage area (30).

2. The production device of a silane coupling agent according to claim 1, characterized in that: A feed port (2121) is provided at the top of the feed zone (10); a scraper (253) is provided around the second filter plate (25) to abut against the side wall of the feed zone (10); an upper end surface of the second baffle plate (24) is flush with an upper end surface of the first baffle plate (23); a stopper (2111) is provided above the side wall of the activated carbon zone (20) to support the second baffle plate (24); a discharge port (2112) and an activated carbon filling port (2116) are provided below the side wall; a sealing cover (2117) is provided on the activated carbon filling port (2116); a filter screen (2113) and a first electric valve (2114) are provided on the discharge port (2112); and a water outlet (2115) is provided at the bottom of the drainage zone (30).

3. The production device of a silane coupling agent according to claim 2, characterized in that: The water-permeable plate (22) is detachably mounted on the upper end surface of the first baffle (23); the first baffle (23) is fixed to the bottom of the shell (21); the shell (21) comprises a shell body (211) with an open top; the shell body (211) is provided with an upper cover (212) on the top and supporting legs (213) on the bottom; the activated carbon zone (20) is provided with a stirring paddle (27); and the bottom of the shell (21) is provided with a motor (28) connected to the stirring paddle (27).

4. The production device of a silane coupling agent according to claim 3, characterized in that: The sealing plug (251) comprises a thin cylindrical section (2511) connected to the second filter plate (25); the bottom of the thin cylindrical section (2511) is connected to a conical section (2512) whose diameter increases downward; the bottom of the conical section (2512) is connected to a thick cylindrical section (2513); and the thick cylindrical section (2513) blocks the through hole (241).

5. The production device of a silane coupling agent according to claim 4, characterized in that: The upper end surface of the second baffle plate (24) is provided with an "inverted L"-shaped first hook (242), and the lower end surface of the second filter plate (25) is provided with an "L"-shaped second hook (252), and the first hook (242) and the second hook (252) are slidably engaged in a vertical direction.

6. The production device of a silane coupling agent according to claim 5, characterized in that: The lifting drive mechanism (26) comprises a liquid storage cylinder (261), the liquid storage cylinder (261) being connected to a vertically arranged hydraulic telescopic sleeve (262), the hydraulic telescopic sleeve (262) being connected to the second filter plate (25); the liquid storage cylinder (261) comprises a sealed cylinder body (2611), a piston (2612) being provided inside the cylinder body (2611), the piston (2612) sealingly separating the cylinder body (2611) into a first hydraulic chamber (2613) and a second hydraulic chamber (2614), the first hydraulic chamber (2613) being provided with a liquid inlet (2615), and the second hydraulic chamber (2614) being connected to the hydraulic telescopic sleeve (262).

7. The production device of a silane coupling agent according to claim 6, characterized in that: The cylinder body (2611) and the piston (2612) are both annular in shape; the cylinder body (2611) is disposed at the bottom of the housing (21); the liquid inlet (2615) is disposed below the side wall of the cylinder body (2611); the piston (2612) is disposed above the liquid inlet (2615); and a support rod (2616) is provided at the bottom.

8. The production device of a silane coupling agent according to claim 6, characterized in that: The hydraulic telescopic sleeve (262) comprises a fixed cylinder (2621) which passes through the housing (21) in a sealed manner, an intermediate slide cylinder (2622) is provided inside the fixed cylinder (2621) in a sealing and sliding manner, a piston rod (2623) is provided inside the intermediate slide cylinder (2622) in a sliding manner, the fixed cylinder (2621) is fixed to the cylinder body (2611) and is in sealed communication with the second hydraulic chamber (2614), the intermediate slide cylinder (2622) comprises a plurality of cylinders which are sealingly and slidingly sleeved, and the piston rod (2623) can pass through the through hole (241) and be connected to the sealing plug (251).

9. The production device of a silane coupling agent according to claim 6, characterized in that: An overflow port (2118) is provided on the side wall of the drainage area (30), the upper end surface of the overflow port (2118) is flush with the upper end surface of the first baffle (23), a connecting pipe (29) is connected to the water outlet (2115) and the liquid inlet (2615), a second electric valve (291) is provided on the connecting pipe (29), a liquid discharge port (2617) is provided at the bottom of the cylinder body (2611), and a third electric valve (2618) is provided on the liquid discharge port (2617).

10. A method for producing a silane coupling agent, characterized in that: The production device for producing a silane coupling agent according to any one of claims 1 to 9 is used for production, comprising the following steps: Step S100, adding measured sodium hydroxide, sulfur and deionized water into the reaction kettle (1), stirring and heating to 50-70° C., and continuing the reaction for 15-30 minutes after the solid is completely dissolved; Step S200, heating the reaction kettle (1) to 75-85°C, adding a measured amount of γ-chloropropyltriethoxysilane dropwise into the reaction kettle (1), and continuing the reaction for 20-30 minutes after the addition is complete, to obtain a crude product of silane coupling agent Si-69; Step S300, cooling the crude product in the reactor (1) to below 40° C., then passing the crude product into the feed zone (10) of the separation device (2), and allowing water in the crude product to flow from the water-permeable plate (22) into the drainage zone (30) for dehydration; Step S400, after dehydration is completed, the lifting drive mechanism (26) drives the second filter plate (25) to slowly rise to the top of the housing (21), and the solid impurities in the dehydrated crude product are trapped on the upper end surface of the second filter plate (25); Step S500, while the second filter plate (25) is rising, the sealing plug (251) is separated from the through hole (241) of the second baffle plate (24), and the crude product after dehydration and filtration enters the activated carbon zone (20) through the through hole (241), and the activated carbon in the activated carbon zone (20) decolorizes the crude product after dehydration and filtration, and a purified product is obtained after the decolorization is completed; Step S600, passing the purified product into a distillation kettle, and obtaining the silane coupling agent Si-69 after negative pressure distillation.

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