A hydrolysis reaction device for producing monoketal
By designing a hydrolysis reaction device for monoketal production, using a central stirring rod and cooling stirring pipe combined with a circulation pump system, the problems of independent equipment and large energy consumption in the existing technology are solved, and the precise control of reaction temperature and heat are achieved. Recycling improves production efficiency.
Patent Information
- Application Number
- CN202411246525.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-06
- Publication Date
- 2024-12-13
- Estimated Expiration
- 2044-09-06
AI Technical Summary
In the existing monoketal production process, condensation reaction and hydrolysis reaction are usually carried out using independent equipment, which requires the control of temperature and material supply parameters separately. In addition, traditional cooling systems use external cooling media, resulting in large energy consumption.
A hydrolysis reaction device for the production of monoketal ketal is designed, including a reactor, a closed reaction chamber, a central stirring rod, a cooling stirring tube and a circulation pump system. The agitation and cooling structure is formed through the central stirring rod and a cooling stirring tube, and a hydrolysis storage tank is used. The circulation system of the condensation storage tank is cooled and preheated to the reaction medium to achieve control of the reaction temperature and heat recovery.
It improves the control accuracy of reaction temperature and overall production efficiency, reduces energy consumption, simplifies the reaction process, and improves the flow efficiency.
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Figure CN118751187B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical production, and in particular to a hydrolysis reaction device for monoketal production. Background Art
[0002] Monoketals are an important class of organic compounds, which are widely used in the fields of medicine, pesticides, dyes and fragrances. Among them, 1,4-cyclohexanedione monoketal is a common monoketal. Its preparation usually involves two main steps: condensation reaction and subsequent hydrolysis reaction. With the development of liquid crystal display technology, the requirements for liquid crystal materials are getting higher and higher. Due to the difficulty in developing new varieties, the transformation of existing liquid crystal materials has become a hot topic in current research. One of them is to replace the benzene ring in the molecule with a cyclohexane ring to reduce the viscosity index of the liquid crystal material. 1,4-cyclohexanedione monoethylene glycol ketal has received more and more attention in the synthesis of cyclohexylbenzene and other liquid crystals.
[0003] In the condensation reaction, DMSS and ethylene glycol are usually used as raw materials, and a condensation reaction is carried out under the action of a catalyst to prepare 1,4-cyclohexanedione diketal. This process usually needs to be carried out at a certain temperature, and the reaction temperature needs to be effectively controlled to improve the selectivity and yield of the reaction. After the condensation reaction is completed, a hydrolysis reaction needs to be carried out, that is, water is used as a solvent, and 1,4-cyclohexanedione diketal is hydrolyzed under the action of a catalyst to prepare 1,4-cyclohexanedione monoketal. This process also requires strict control of the reaction temperature. However, in the current existing monoketal production process, the condensation reaction and the hydrolysis reaction are usually carried out using independent equipment, and the temperature, material supply and other parameters of the two reactions need to be controlled separately. In addition, the traditional cooling system usually uses an external cooling medium, which consumes a lot of energy. Summary of the invention
[0004] In view of this, the purpose of the present invention is to propose a hydrolysis reaction device for monoketal production to solve the problem that in the current monoketal production process, the condensation reaction and the hydrolysis reaction are usually carried out using independent equipment, and the temperature, material supply and other parameters of the two reactions need to be controlled separately, and the traditional cooling system usually uses an external cooling medium, which consumes a lot of energy.
[0005] Based on the above purpose, the present invention provides a hydrolysis reaction device for monoketal production, including a reactor, wherein a closed reaction chamber is provided inside the reactor, and further comprising:
[0006] A closed sleeve is arranged at the center of the top and bottom of the reactor, a central stirring rod is nested and rotatably arranged inside the closed sleeve, a central input pipe is arranged at the inner top of the central stirring rod, and a central output pipe is arranged at the inner bottom of the central stirring rod;
[0007] An input three-way valve is connected to the top of the central input pipe. The central input pipe and the input three-way valve are rotatably connected to each other through a rotating joint arranged therebetween. The left and right sides of the input three-way valve are respectively connected to a first input pipe and a second input pipe. The outer ends of the first input pipe and the second input pipe are respectively connected to a hydrolysis storage tank and a condensation storage tank;
[0008] An output three-way valve is connected to the bottom end of the central output pipe, the central output pipe and the output three-way valve are rotatably connected to each other through a rotary joint arranged therebetween, the left and right sides of the output three-way valve are respectively connected to a first output pipe and a second output pipe, the outer ends of the first output pipe and the second output pipe are respectively connected to the hydrolysis storage tank and the condensation storage tank, and the middle of the first output pipe and the second output pipe are respectively connected to a first circulation pump and a second circulation pump;
[0009] A plurality of cooling stirring tubes are evenly connected and arranged in a circular shape around the outside of the central stirring rod, and the top and bottom ends of the cooling stirring tubes are respectively connected to the central input tube and the central output tube.
[0010] Furthermore, the outer openings of the first input pipe and the first output pipe are both located at the bottom of the hydrolysis storage tank, the outer openings of the second input pipe and the second output pipe are respectively located at the bottom of the condensation storage tank, and the top ends of the hydrolysis storage tank and the condensation storage tank are respectively connected with a hydrolysis feeding pipe and a condensation feeding pipe.
[0011] Furthermore, the central stirring rod is rotatably connected to the reactor through the closed shaft sleeve, a rotating gear ring is arranged around the top end of the central stirring rod, a rotating gear is meshed on the outer side of the rotating gear ring, a stirring motor is connected to the shaft end of the rotating gear, and the stirring motor is fixedly connected to the reactor.
[0012] Furthermore, one-way conveying valves are provided at the top and bottom ends of the cooling stirring tube respectively connected to the central input tube and the central output tube. The conveying direction of the one-way conveying valve provided at the connection between the cooling stirring tube and the central input tube is from the central input tube to the cooling stirring tube, and the conveying direction of the one-way conveying valve provided at the connection between the cooling stirring tube and the central output tube is from the cooling stirring tube to the central output tube.
[0013] Furthermore, a plurality of cooling fins are disposed around and connected to the outer side of the cooling and stirring tube, and the plurality of cooling fins are evenly arranged in parallel along the vertical center line direction of the cooling and stirring tube, and a plurality of drag-reducing holes are evenly disposed in the middle of the cooling fins.
[0014] Furthermore, a plurality of interlocking grooves are evenly arranged around the outer wall of the cooling stirring tube, the interlocking grooves and the cooling stirring tube are arranged parallel to each other, an interlocking sleeve is arranged at the center of the cooling fin, a plurality of interlocking sliders are evenly arranged around the inner side of the interlocking sleeve, the interlocking sliders and the interlocking grooves are arranged corresponding to each other, and the cooling fins are slidably connected to the cooling stirring tube through the interlocking sleeve.
[0015] Furthermore, a spacing spring is arranged between the interlocking sleeves of adjacent cooling fins, a synchronous connecting frame is symmetrically arranged on the top and bottom of the cooling and stirring tube, a plurality of connecting sleeves are arranged around the middle of the synchronous connecting frame, the connecting sleeves and the cooling and stirring tube are arranged corresponding to each other, the synchronous connecting frame is slidingly connected to all cooling and stirring tubes through the connecting sleeves, a synchronous adjustment frame is rotatably connected around the outer side of the synchronous connecting frame, lifting screws are arranged on both sides of the inner side of the closed reaction chamber, a lifting motor is connected to the axial end of the lifting screw, and lifting screw sleeves are arranged in the middle of the synchronous adjustment frames symmetrically arranged up and down, and the synchronous adjustment frames symmetrically arranged up and down are respectively connected to the lifting screws symmetrically arranged on the left and right through the lifting screw sleeves.
[0016] Furthermore, a central feeding pipe is arranged in the middle of the inner side of the central stirring rod, and a plurality of horizontal feeding pipes are evenly arranged and connected on the outer side of the central feeding pipe, and the plurality of horizontal feeding pipes are evenly arranged along the vertical center line direction of the central feeding pipe, and a plurality of feeding openings are evenly arranged along the horizontal direction on the outer wall of the horizontal feeding pipe, and the feeding openings are interconnected with the central feeding pipe through the horizontal feeding pipe, and a spacer sealing plate is arranged between the top end of the central feeding pipe and the central input pipe, and a feeding one-way valve is arranged between the bottom end of the central feeding pipe and the central output pipe, and the passing direction of the feeding one-way valve is from the central output pipe to the central feeding pipe.
[0017] Furthermore, a rotating sleeve is nested and rotatably arranged on the outer side of the horizontal feeding pipe, a spiral groove is arranged through the middle of the outer wall of the rotating sleeve, and a plurality of arc-shaped blades are evenly arranged around the outer side of the rotating sleeve.
[0018] Furthermore, a limiting piston is nested and slidably arranged on the inner side of the horizontal feeding pipe, a guide sleeve and an adjusting screw sleeve are arranged in the middle of the limiting piston, a fixed guide rod and an adjusting screw sleeve are nested and connected on the inner sides of the guide sleeve and the adjusting screw sleeve respectively, the fixed guide rod and the adjusting screw are interconnected with the horizontal feeding pipe, and an adjusting motor is connected to the axial end of the adjusting screw.
[0019] Beneficial effects of the present invention: As can be seen from the above description, a hydrolysis reaction device for monoketal production provided by the present invention forms a stirring and cooling structure through a central stirring rod and a cooling stirring tube. At the same time, the raw water required for the subsequent hydrolysis reaction and the ethylene glycol required for the storage reaction are respectively stored through a hydrolysis storage tank and a condensation storage tank, and the hydrolysis storage tank and the condensation storage tank are interconnected with the cooling stirring tube through an independent circulation system. During the condensation reaction and the hydrolysis reaction, the raw materials required for another reaction are used to cool the reaction through an adjustable cooling system, which can not only control the temperature of the ongoing reaction, but also preheat the raw materials required for the subsequent reaction to recover the reaction heat, which is beneficial to improving the overall production flow efficiency and is more convenient and energy-saving during the overall reaction processing. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] In order to more clearly illustrate the technical solutions in the present invention or 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 in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0021] Figure 1 It is a front structural schematic diagram of an embodiment of the present invention;
[0022] Figure 2 It is a schematic diagram of the longitudinal cross-sectional structure of an embodiment of the present invention;
[0023] Figure 3 It is a structural schematic diagram of a reactor according to an embodiment of the present invention;
[0024] Figure 4 A schematic diagram of the internal structure of a reactor according to an embodiment of the present invention;
[0025] Figure 5 A schematic structural diagram of a central stirring rod according to an embodiment of the present invention;
[0026] Figure 6 This is a schematic structural diagram of a cooling and stirring tube according to an embodiment of the present invention;
[0027] Figure 7 It is a schematic structural diagram of a cooling fin according to an embodiment of the present invention;
[0028] Figure 8 It is a schematic structural diagram of a horizontal feeding pipe according to an embodiment of the present invention.
[0029] The markings in the figure are:
[0030] 1. Reactor; 101. Closed reaction chamber; 102. Feeding interface; 103. Discharging interface; 2. Closed sleeve; 201. Central stirring rod; 202. Rotating gear ring; 203. Rotating gear; 204. Stirring motor; 205. Central feeding pipe; 206. Interval closing plate; 207. Feeding one-way valve; 3. Cooling stirring pipe; 301. One-way delivery valve; 302. Embedded slide groove; 303. Cooling fin; 304. Drag reduction hole; 305. Embedded sleeve; 306. Embedded slider; 307. Interval spring; 4. Synchronous connecting frame; 401. Connecting sleeve; 402. Synchronous adjustment frame; 403. Lifting screw sleeve; 404. Lifting screw; 405. Lifting motor; 5. Central Central input tube; 501, central output tube; 502, rotary joint; 503, input three-way valve; 504, output three-way valve; 6, first input tube; 601, first output tube; 602, first circulation pump; 603, hydrolysis storage tank; 604, hydrolysis feeding tube; 7, second input tube; 701, second output tube; 702, second circulation pump; 703, condensation storage tank; 704, condensation feeding tube; 8, horizontal feeding tube; 801, feeding opening; 802, rotary sleeve; 803, arc blade; 804, spiral groove; 9, limit piston; 901, guide sleeve; 902, adjusting screw sleeve; 903, fixed guide rod; 904, adjusting screw; 905, adjusting motor. DETAILED DESCRIPTION
[0031] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.
[0032] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.
[0033] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 As shown, a hydrolysis reaction device for monoketal production includes a reactor 1, wherein a closed reaction chamber 101 is provided inside the reactor 1, and further includes:
[0034] The closed sleeve 2 is arranged at the center of the top and bottom of the reactor 1, and a central stirring rod 201 is nested and rotatably arranged inside the closed sleeve 2. A central input pipe 5 is arranged at the inner top of the central stirring rod 201, and a central output pipe 501 is arranged at the inner bottom of the central stirring rod 201;
[0035] An input three-way valve 503 is connected to the top of the central input pipe 5. The central input pipe 5 and the input three-way valve 503 are rotatably connected to each other via a rotary joint 502 arranged therebetween. The left and right sides of the input three-way valve 503 are respectively connected to a first input pipe 6 and a second input pipe 7. The outer ends of the first input pipe 6 and the second input pipe 7 are respectively connected to a hydrolysis storage tank 603 and a condensation storage tank 703.
[0036] An output three-way valve 504 is connected to the bottom end of the central output pipe 501. The central output pipe 501 and the output three-way valve 504 are rotatably connected to each other via a rotary joint 502 arranged therebetween. The left and right sides of the output three-way valve 504 are respectively connected to a first output pipe 601 and a second output pipe 701. The outer ends of the first output pipe 601 and the second output pipe 701 are respectively connected to a hydrolysis storage tank 603 and a condensation storage tank 703. A first circulation pump 602 and a second circulation pump 702 are respectively connected to the middle of the first output pipe 601 and the second output pipe 701.
[0037] The cooling stirring tubes 3 are evenly connected and arranged in a circular shape on the outside of the central stirring rod 201 . The top and bottom ends of the cooling stirring tubes 3 are respectively connected to the central input tube 5 and the central output tube 501 .
[0038] In this embodiment, when the device is in production, DMSS and ethylene glycol are first used as raw materials. Under the action of a catalyst, a condensation reaction is carried out in a closed reaction chamber 101 arranged inside the reactor 1 to prepare 1,4-cyclohexanedione bisketal. During the reaction, the central stirring rod 201 drives multiple cooling stirring tubes 3 to mix and stir the reactants to improve the reaction uniformity. At the same time, the device stores the raw water required for the subsequent hydrolysis reaction through the hydrolysis storage tank 603. Since the condensation reaction process is exothermic, the reactants need to be cooled to maintain them at a suitable reaction temperature to avoid excessive temperature affecting the reaction effect. Therefore, when the condensation reaction is carried out, the input three-way valve 503 is used to adjust and control the connection between the first input pipe 6 and the central input pipe. 5, the central output pipe 501 and the first output pipe 601 are connected through the output three-way valve 504, and then the first circulation pump 602 pumps the raw water stored in the hydrolysis storage tank 603 through the first input pipe 6 and the input three-way valve 503 to the central input pipe 5, and then uniformly transports it to all the cooling and stirring pipes 3, and then transports it to the central output pipe 501 through the cooling and stirring pipes 3, and then refluxes through the central output pipe 501, the output three-way valve 504 and the first output pipe 601 to the hydrolysis storage tank 603. In this process, the internal reactants can be cooled by water to maintain a suitable reaction temperature. At the same time, since the cooling and stirring pipe 3 is synchronously rotated and stirred when transporting the cooling medium, the heat exchange efficiency can be improved to improve The cooling efficiency is improved. After the condensation reaction is completed, water is used as a solvent to hydrolyze 1,4-cyclohexanedione diketal under the action of a catalyst to prepare 1,4-cyclohexanedione monoketal. The raw water cooled during the condensation reaction absorbs a certain amount of heat and can be transported through the feeding interface 102 set on the top of the reactor 1 to the reactor 1 for reaction. This avoids directly adding water with a lower temperature, which causes the temperature of the reactants to drop and the fluidity to decrease. This is beneficial to maintaining the temperature and fluidity of the reactants and facilitating the start of the hydrolysis reaction as soon as possible. During the hydrolysis reaction, the ethylene glycol required for the reaction is stored in the condensation storage tank 703. The hydrolysis reaction process is also an exothermic reaction, and the reactants need to be cooled to maintain them at a suitable temperature. The reaction temperature is to avoid the reaction effect being affected by excessive temperature, so that at this time, the second input pipe 7 and the central input pipe 5 are connected by adjusting and controlling through the input three-way valve 503, and the central output pipe 501 and the second output pipe 701 are connected through the output three-way valve 504, and then the second circulation pump 702 transports the stored ethylene glycol to the central input pipe 5 through the second input pipe 7 and the input three-way valve 503, and further transports it to multiple cooling and stirring pipes 3, and then transports it to the central output pipe 501 through the cooling and stirring pipe 3 and the second output pipe 701, and then refluxes through the central output pipe 501 and the output three-way valve 504 to the condensation storage tank 703. In this process, the internal reactants can be cooled by ethylene glycol, and the raw material ethylene glycol can be heated at the same time.It is convenient to maintain the temperature and fluidity of the reactants during the subsequent condensation reaction, so as to start the reaction as soon as possible. Therefore, during the condensation reaction and hydrolysis reaction, the device uses the raw materials required for another reaction to cool the reaction through an adjustable cooling system. It can not only control the temperature of the ongoing reaction, but also preheat the raw materials required for the subsequent reaction to recover the reaction heat, which is beneficial to improve the overall production flow efficiency and is more convenient and energy-saving during the overall reaction processing.
[0039] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 As shown, preferably, the outer end openings of the first input pipe 6 and the first output pipe 601 arranged in the device are both located at the bottom of the hydrolysis storage tank 603, and the outer end openings of the second input pipe 7 and the second output pipe 701 are respectively located at the bottom of the condensation storage tank 703, and the tops of the hydrolysis storage tank 603 and the condensation storage tank 703 are respectively connected with the hydrolysis feeding pipe 604 and the condensation feeding pipe 704, so as to facilitate the circulation and cooling of the raw materials. At the same time, the central stirring rod 201 is rotatably connected to the reactor 1 through the closed shaft sleeve 2, and the top of the central stirring rod 201 is surrounded by a rotating gear ring 202, and the outer side of the rotating gear ring 202 is meshed with a rotating gear 203, and the shaft end of the rotating gear 203 is connected with a stirring motor 204, and the stirring motor 204 is fixedly connected to the reactor 1, so that the stirring motor 204 can drive the central stirring rod 201 to rotate through the rotating gear 203 and the rotating gear ring 202, thereby driving multiple cooling stirring tubes 3 to mix and stir the reactants to improve the reaction uniformity.
[0040] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 As shown, preferably, one-way delivery valves 301 are provided at the top and bottom ends of the cooling and stirring tube 3 of the device respectively connecting with the central input tube 5 and the central output tube 501. The one-way delivery valve 301 provided at the connection between the cooling and stirring tube 3 and the central input tube 5 has a delivery direction from the central input tube 5 to the cooling and stirring tube 3, and the one-way delivery valve 301 provided at the connection between the cooling and stirring tube 3 and the central output tube 501 has a delivery direction from the cooling and stirring tube 3 to the central output tube 501, thereby facilitating the continuous circulation delivery of the reaction raw materials to cool the reactants.
[0041] like Figure 1 , Figure 2, Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 As shown, preferably, a plurality of cooling fins 303 are arranged around and connected to the outer side of the cooling and stirring tube 3 of the device, and the plurality of cooling fins 303 are evenly arranged in parallel along the vertical center line direction of the cooling and stirring tube 3, so that the relative surface area of the cooling and stirring tube 3 can be increased by the plurality of cooling fins 303 to improve the heat exchange and cooling efficiency, and a plurality of drag reduction holes 304 are evenly arranged in the middle of the cooling fins 303, which is conducive to further increasing the relative surface area and reducing the blocking area of the cooling fins 303 to reduce the rotational resistance of the cooling and stirring tube 3, and at the same time, a plurality of interlocking grooves 302 are evenly arranged around the outer wall of the cooling and stirring tube 3, and the interlocking grooves 302 and the cooling and stirring tube 3 are arranged parallel to each other, and an interlocking sleeve 305 is arranged at the center of the cooling fin 303, and an interlocking sleeve 305 is evenly arranged on the inner side thereof. A plurality of interlocking sliders 306 are arranged corresponding to the interlocking slide grooves 302, thereby increasing the contact area between the interlocking sleeve 305 and the cooling and stirring tube 3, and further increasing the heat exchange efficiency between the cooling fins 303, the interlocking sleeve 305 and the cooling and stirring tube 3. At the same time, the cooling fins 303 are slidably connected to the cooling and stirring tube 3 through the interlocking sleeve 305, so that the cooling fins 303 can slide up and down to adjust the position and height, so as to adjust the liquid level inside the reactor 1, so that the cooling fins 303 can be completely immersed under the liquid surface, thereby improving the heat exchange and cooling efficiency, or adjusting the number of cooling fins 303 immersed under the liquid surface, so as to adjust the cooling efficiency according to the data of the temperature sensor arranged inside the closed reaction chamber 101, so as to control the temperature of the reactants, which is more convenient and flexible to use.
[0042] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8As shown, preferably, a spacing spring 307 is arranged between the interlocking sleeves 305 of adjacent cooling fins 303 of the device, a synchronous connecting frame 4 is symmetrically arranged on the top and bottom of the cooling stirring tube 3, a plurality of connecting sleeves 401 are arranged around the middle of the synchronous connecting frame 4, the connecting sleeves 401 and the cooling stirring tube 3 are arranged correspondingly to each other, the synchronous connecting frame 4 is slidably connected to all the cooling stirring tubes 3 through the connecting sleeves 401, a synchronous adjustment frame 402 is arranged around the outer side of the synchronous connecting frame 4 for rotational connection, lifting screws 404 are arranged on both sides of the inside of the closed reaction chamber 101, and a lifting motor 405 is connected to the shaft end of the lifting screw 404, which is symmetrically arranged up and down. A lifting screw sleeve 403 is provided in the middle of the synchronous adjustment frame 402. The synchronous adjustment frames 402 symmetrically arranged up and down are respectively connected to the lifting screw rods 404 symmetrically arranged left and right through the lifting screw sleeves 403, so that the lifting motor 405 can drive the corresponding synchronous adjustment frame 402 to move up and down through the lifting screw rods 404 and the lifting screw sleeves 403, and then the synchronous adjustment frame 402 drives the synchronous connecting frame 4 to move up and down to squeeze the cooling fins 303 to slide up and down, so that the positions and heights of all cooling fins 303 can be adjusted through the coordinated movement of the synchronous connecting frames 4 on the upper and lower sides, so as to facilitate the adjustment according to the internal liquid level height and demand of the reactor 1, which is more convenient and flexible to use.
[0043] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8As shown, preferably, a central feeding pipe 205 is arranged in the middle of the inner side of the central stirring rod 201 of the device, and a spacer sealing plate 206 is arranged between the top of the central feeding pipe 205 and the central input pipe 5, so that the first circulating pump 602 and the second circulating pump 702 arranged in the device are both bidirectional conveying pumps. When cooling is performed, the circulation conveying direction of the first circulating pump 602 and the second circulating pump 702 is to convey from the central input pipe 5 to the cooling stirring pipe 3, and then to the central output pipe 501. When feeding is required, the raw materials are conveyed to the bottom of the cooling stirring pipe 3 through the central output pipe 501. At the end connection, since a one-way delivery valve 301 is provided at the bottom end of the cooling and stirring tube 3, the raw material cannot be delivered to the cooling and stirring tube 3, and a feeding one-way valve 207 is provided between the bottom end of the central feeding tube 205 and the central output tube 501, and the passing direction of the feeding one-way valve 207 is from the central output tube 501 to the central feeding tube 205, so that the raw material can be delivered to the inside of the central feeding tube 205, and a plurality of horizontal feeding tubes 8 are uniformly arranged around the outer side of the central feeding tube 205, and the plurality of horizontal feeding tubes 8 are uniformly arranged along the vertical center line direction of the central feeding tube 205. The outer wall of the horizontal feeding pipe 8 is evenly arranged with a plurality of feeding openings 801 in the horizontal direction, and the feeding openings 801 are interconnected with the central feeding pipe 205 through the horizontal feeding pipe 8, so that the raw materials can be evenly transported to the plurality of horizontal feeding pipes 8, and transported to the inside of the closed reaction chamber 101 through the feeding openings 801, so as to complete the automatic feeding of the raw materials, which is more convenient and uniform when feeding, and is conducive to improving the reaction production efficiency, and the outer side of the horizontal feeding pipe 8 is nested and rotatably provided with a rotating sleeve 802, and the outer wall of the rotating sleeve 802 is penetrated by a spiral spiral groove 808. 04. A plurality of arc-shaped blades 803 are evenly arranged around the outer side of the rotating sleeve 802. When the central stirring rod 201 drives the horizontal feeding tube 8 to rotate, the arc-shaped blades 803 on the rotating sleeve 802 are impacted by the reverse force of the liquid, which can drive the rotating sleeve 802 to rotate, and then drive the spiral groove 804 to rotate. The spiral groove 804 and the corresponding feeding opening 801 are arranged in cooperation with each other. When the spiral groove 804 and the feeding opening 801 overlap with each other, the feeding opening 801 can be opened to convey the raw materials, thereby further improving the uniformity of the added raw materials.
[0044] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8As shown, preferably, a limit piston 9 is nested and slidably arranged on the inner side of the horizontal feeding pipe 8 of the device, and a guide sleeve 901 and an adjusting screw sleeve 902 are arranged in the middle of the limit piston 9, and a fixed guide rod 903 and an adjusting screw 904 are nested and connected on the inner sides of the guide sleeve 901 and the adjusting screw sleeve 902 respectively, and the fixed guide rod 903 and the adjusting screw 904 are interconnected with the horizontal feeding pipe 8, and an adjusting motor 905 is connected to the axial end of the adjusting screw 904, so that the adjusting motor 905 can drive the limit piston 9 to move up and down through the adjusting screw 904 and the adjusting screw sleeve 902 to adjust the height of the limit piston 9, so that the distance that the raw material is conveyed upward along the central feeding pipe 205 can be adjusted, and then the height and amount of the raw material that can be conveyed to the horizontal feeding pipe 8 can be adjusted to ensure that the raw material can be directly conveyed below the liquid surface, thereby improving the uniformity of raw material conveying.
[0045] When in use, first connect the corresponding pipelines of the device, then add DMSS, ethylene glycol and the catalyst into the closed reaction chamber 101 through the feeding interface 102, and under the action of the catalyst, a condensation reaction is carried out in the closed reaction chamber 101 arranged inside the reactor 1 to prepare 1,4-cyclohexanedione bisacetal. During the reaction, the stirring motor 204 drives the central stirring rod 201 to rotate through the rotating gear 203 and the rotating gear ring 202, and then the central stirring rod 201 drives the multiple cooling stirring tubes 3 to mix and stir the reactants to improve the reaction uniformity. At the same time, the device stores the raw water required for the subsequent hydrolysis reaction through the arranged hydrolysis storage tank 603. The condensation reaction process is exothermic. When the condensation reaction is carried out, the first input pipe 6 and the central input pipe 5 are connected by adjusting and controlling the input three-way valve 503, and the central output pipe 501 and the first output pipe 601 are connected by the output three-way valve 504. Then the first circulation pump 602 pumps the raw water stored in the hydrolysis storage tank 603 through the first input pipe 6 and the input three-way valve 503 to the central input pipe 5, and then uniformly transports it to all the cooling and stirring pipes 3, and then transports it to the central output pipe 501 through the cooling and stirring pipe 3, and then refluxes it to the hydrolysis storage tank 603 through the central output pipe 501, the output three-way valve 504 and the first output pipe 601. In this process, The internal reactants are cooled by water to maintain a suitable reaction temperature. After the condensation reaction is completed, the first circulation pump 602 transports the raw water to the central input pipe 5 through the first output pipe 601 and the output three-way valve 504, and then transports it to the inside of the central feeding pipe 205. The raw materials can be uniformly transported to multiple horizontal feeding pipes 8, and transported to the inside of the closed reaction chamber 101 through the feeding opening 801, so that 1,4-cyclohexanedione diketal is hydrolyzed with water as a solvent under the action of a catalyst to prepare 1,4-cyclohexanedione monoketal. During the hydrolysis reaction, the second input pipe 7 and the central input pipe 5 are connected by adjusting and controlling the input three-way valve 503, and the output is connected by adjusting and controlling the output three-way valve 503. The outlet three-way valve 504 connects the central output pipe 501 and the second output pipe 701, and then the second circulation pump 702 transports the stored ethylene glycol to the central input pipe 5 through the second input pipe 7 and the input three-way valve 503, and further transports it to multiple cooling and stirring pipes 3, and then transports it to the central output pipe 501 through the cooling and stirring pipes 3 and the second output pipe 701, and then refluxes through the central output pipe 501 and the output three-way valve 504 to the condensation storage tank 703. In this process, the internal reactants can be cooled by ethylene glycol, and the raw material ethylene glycol can be heated at the same time. After the reaction is completed, the reaction product is output through the discharge interface 103 set at the bottom of the reactor 1.
[0046] The hydrolysis reaction device for monoketal production provided by the present invention forms a stirring and cooling structure through a central stirring rod 201 and a cooling stirring tube 3. At the same time, the raw water required for the subsequent hydrolysis reaction and the ethylene glycol required for the storage reaction are respectively stored through a hydrolysis storage tank 603 and a condensation storage tank 703, and the hydrolysis storage tank 603 and the condensation storage tank 703 are interconnected with the cooling stirring tube 3 through an independent circulation system. During the condensation reaction and the hydrolysis reaction, the raw materials required for the other reaction are used to cool the reaction through an adjustable cooling system, which can not only control the temperature of the ongoing reaction, but also preheat the raw materials required for the subsequent reaction to recover the reaction heat, which is beneficial to improving the overall production flow efficiency and is more convenient and energy-saving during the overall reaction processing.
[0047] Those skilled in the art should understand that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of the present invention is limited to these examples; under the concept of the present invention, the technical features in the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other changes in different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity. Any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A hydrolysis reaction device for producing monoketal, comprising a reaction kettle (1), wherein a closed reaction chamber (101) is arranged inside the reaction kettle (1), characterized in that: Also includes: A closed shaft sleeve (2) is arranged at the center of the top and bottom of the reactor (1); a central stirring rod (201) is nested and rotatably arranged inside the closed shaft sleeve (2); a central input pipe (5) is arranged at the inner top of the central stirring rod (201); and a central output pipe (501) is arranged at the inner bottom of the central stirring rod (201); An input three-way valve (503) is connected to the top of the central input pipe (5); the central input pipe (5) and the input three-way valve (503) are rotatably connected to each other via a rotary joint (502) arranged therebetween; the left and right sides of the input three-way valve (503) are respectively connected to a first input pipe (6) and a second input pipe (7); the outer ends of the first input pipe (6) and the second input pipe (7) are respectively connected to a hydrolysis storage tank (603) and a condensation storage tank (703); An output three-way valve (504) is connected to the bottom end of the central output pipe (501); the central output pipe (501) and the output three-way valve (504) are rotatably connected to each other via a rotary joint (502) arranged therebetween; the left and right sides of the output three-way valve (504) are respectively connected to a first output pipe (601) and a second output pipe (701); the outer ends of the first output pipe (601) and the second output pipe (701) are respectively connected to the hydrolysis storage tank (603) and the condensation storage tank (703); the middle of the first output pipe (601) and the second output pipe (701) are respectively connected to a first circulation pump (602) and a second circulation pump (702); A cooling stirring tube (3), wherein a plurality of cooling stirring tubes (3) are evenly connected and arranged in a circular shape around the outside of the central stirring rod (201), and the top and bottom ends of the cooling stirring tube (3) are respectively connected to the central input tube (5) and the central output tube (501); A central feeding pipe (205) is arranged in the middle of the inner side of the central stirring rod (201), and a plurality of horizontal feeding pipes (8) are evenly arranged and connected to the outer side of the central feeding pipe (205). The plurality of horizontal feeding pipes (8) are evenly arranged along the vertical center line direction of the central feeding pipe (205). The outer wall of the horizontal feeding pipe (8) is evenly arranged along the horizontal direction with a plurality of feeding openings (801). The feeding openings (801) are interconnected with the central feeding pipe (205) through the horizontal feeding pipe (8). A spacing sealing plate (206) is arranged between the top end of the central feeding pipe (205) and the central input pipe (5). A feeding one-way valve (207) is arranged between the bottom end of the central feeding pipe (205) and the central output pipe (501). The passing direction of the feeding one-way valve (207) is from the central output pipe (501) to the central feeding pipe (205). A rotating sleeve (802) is nested and rotatably arranged on the outer side of the horizontal feeding pipe (8), a spiral groove (804) is arranged through the middle of the outer wall of the rotating sleeve (802), and a plurality of arc-shaped blades (803) are evenly arranged around the outer side of the rotating sleeve (802); A limit piston (9) is nested and slidably arranged inside the horizontal feeding pipe (8), a guide sleeve (901) and an adjusting screw sleeve (902) are arranged in the middle of the limit piston (9), a fixed guide rod (903) and an adjusting screw (904) are nested and connected inside the guide sleeve (901) and the adjusting screw sleeve (902), the fixed guide rod (903) and the adjusting screw (904) are both interconnected with the horizontal feeding pipe (8), and an adjusting motor (905) is connected to the axial end of the adjusting screw (904); One-way conveying valves (301) are provided at the top and bottom ends of the cooling and stirring tube (3) respectively connected to the central input tube (5) and the central output tube (501). The one-way conveying valve (301) provided at the connection between the cooling and stirring tube (3) and the central input tube (5) has a conveying direction from the central input tube (5) to the cooling and stirring tube (3). The one-way conveying valve (301) provided at the connection between the cooling and stirring tube (3) and the central output tube (501) has a conveying direction from the cooling and stirring tube (3) to the central output tube (501).
2. The hydrolysis reaction device for monoketal production according to claim 1, characterized in that: The outer openings of the first input pipe (6) and the first output pipe (601) are both located at the bottom of the hydrolysis storage tank (603), and the outer openings of the second input pipe (7) and the second output pipe (701) are respectively located at the bottom of the condensation storage tank (703), and the top ends of the hydrolysis storage tank (603) and the condensation storage tank (703) are respectively connected to a hydrolysis feeding pipe (604) and a condensation feeding pipe (704).
3. The hydrolysis reaction device for monoketal production according to claim 1, characterized in that: The central stirring rod (201) is rotatably connected to the reactor (1) via the closed shaft sleeve (2); a rotating gear ring (202) is disposed around the top end of the central stirring rod (201); a rotating gear (203) is meshedly disposed on the outer side of the rotating gear ring (202); a stirring motor (204) is connected to the shaft end of the rotating gear (203); and the stirring motor (204) is fixedly connected to the reactor (1).
4. The hydrolysis reaction device for monoketal production according to claim 1, characterized in that: A plurality of cooling fins (303) are arranged around and connected to the outer side of the cooling and stirring tube (3); the plurality of cooling fins (303) are evenly arranged in parallel along the vertical center line direction of the cooling and stirring tube (3); and a plurality of drag reduction holes (304) are evenly arranged in the middle of the cooling fins (303).
5. The hydrolysis reaction device for monoketal production according to claim 4, characterized in that: The outer wall of the cooling and stirring tube (3) is evenly arranged with a plurality of interlocking grooves (302), the interlocking grooves (302) and the cooling and stirring tube (3) are arranged parallel to each other, an interlocking sleeve (305) is arranged at the center of the cooling fin (303), and a plurality of interlocking sliders (306) are evenly arranged on the inner side of the interlocking sleeve (305), the interlocking sliders (306) and the interlocking grooves (302) are arranged corresponding to each other, and the cooling fin (303) is slidably connected to the cooling and stirring tube (3) through the interlocking sleeve (305).
6. The hydrolysis reaction device for monoketal production according to claim 5, characterized in that: A spacing spring (307) is arranged between the interlocking sleeves (305) of adjacent cooling fins (303); a synchronous connecting frame (4) is symmetrically arranged at the top and bottom of the cooling stirring tube (3); a plurality of connecting sleeves (401) are arranged around the middle of the synchronous connecting frame (4); the connecting sleeves (401) and the cooling stirring tube (3) are arranged corresponding to each other; the synchronous connecting frame (4) is slidably connected to all the cooling stirring tubes (3) through the connecting sleeves (401); the synchronous connecting frame (4) is provided with a synchronous adjustment frame (402) which is rotatably connected to the outside, and lifting screws (404) are provided on both sides of the inside of the closed reaction chamber (101), and the shaft ends of the lifting screws (404) are connected with lifting motors (405), and lifting screw sleeves (403) are provided in the middle of the synchronous adjustment frames (402) which are symmetrically arranged up and down, and the synchronous adjustment frames (402) which are symmetrically arranged up and down are respectively connected to the lifting screws (404) which are symmetrically arranged on the left and right through the lifting screw sleeves (403).
Citation Information
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