Preparation method and preparation equipment of dialkyl hypophosphorous acid
By designing a dual-channel intermittent feeding system in the reactor, the safety hazards during raw material addition were solved, safe raw material feeding and reaction control were achieved, gas escape was avoided, and the safety and controllability of the reaction were improved.
Patent Information
- Application Number
- CN202310602395.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-26
- Publication Date
- 2026-02-10
- Estimated Expiration
- 2043-05-26
AI Technical Summary
Adding raw materials to the reactor can easily lead to dangerous problems.
Sodium hypophosphite and diisobutylene are introduced into two cavities through two channels respectively. The rotation of the drive disc moves the cavities and gradually feeds them intermittently towards the feed port. The extrusion plate forces the gas in the cavity back into the main body to prevent gas from escaping, thus achieving small-batch, multiple-time reactions.
This process ensures safe raw material feeding, avoids violent reactions and gas escape, and improves the safety and controllability of the reaction.
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Figure CN116606317B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of dialkyl phosphinic acid preparation, in particular to a dialkyl phosphinic acid preparation method and preparation equipment thereof. BACKGROUND
[0002] Dialkyl phosphinic acid is an acid non-ferrous metal extractant, commonly used for extracting cobalt and nickel.
[0003] According to the disclosure (announcement) No. CN102268038A, the disclosure (announcement) date is December 7, 2011, and the disclosed synthesis method of bis (2, 4, 4-trimethyl pentyl) phosphinic acid is prepared by using sodium hypophosphite and diisobutene as raw materials and acetic acid as a solvent, and the method is characterized by comprising the following steps: 1) dissolving sodium hypophosphite in acetic acid, adding diisobutene, then adding free radical initiator azobis diisobutyl amidine hydrochloride and hydrogen peroxide in the above solution, heating to 60-100°C under stirring, and constant temperature reaction for 3-5h under normal pressure; wherein, the molar ratio of diisobutene to sodium hypophosphite is not less than 5, the molar ratio of acetic acid to sodium hypophosphite is not less than 1, the molar ratio of azobis diisobutyl amidine hydrochloride to sodium hypophosphite is not less than 0.5, and the molar ratio of azobis diisobutyl amidine hydrochloride to sodium hypophosphite is not less than 0.5; 2) standing, separating, washing the organic phase with water, and vacuum distillation to obtain the target product bis (2, 4, 4-trimethyl pentyl) phosphinic acid. The method has the advantages of no need for pressurization, short reaction time, high conversion rate, high product purity, non-toxic decomposition product, and simple post-treatment method.
[0004] In the prior art including the above-mentioned patent, when dialkyl phosphinic acid is prepared by using sodium hypophosphite and diisobutene as raw materials, the two raw materials need to be placed in the reaction kettle in turn for chemical reaction. In order to ensure that the raw materials are completely reacted, intermittent feeding is required. However, the internal raw materials of the reaction kettle need to be heated during the reaction, so the internal pressure of the reaction kettle is very high, and danger is easy to occur when the raw materials are added. SUMMARY
[0005] The purpose of the present application is to provide a dialkyl phosphinic acid preparation method and preparation equipment, which aims to solve the problem of danger in adding raw materials to the reaction kettle during the reaction.
[0006] In order to achieve the above-mentioned purpose, the present application provides a dialkyl phosphinic acid preparation method, which comprises the following steps:
[0007] S1, sodium hypophosphite and diisobutene are respectively introduced into two cavities through two channels;
[0008] S2, the driving disc is driven to rotate to drive one of the cavities to move and gradually face the discharge port, the discharge port is opened, and the raw materials in the cavity are introduced into the body;
[0009] S3. The extrusion plate inside the cavity moves downward, pressing the air that has escaped from the main body back into the main body;
[0010] S4. The drive disc is driven to rotate in the opposite direction, so that the cavity returns to its initial position, and the other cavity gradually faces the feeding port to feed the material.
[0011] S5. When the cavity moves to the initial position, the extrusion plate is driven to move upward, opening the cavity;
[0012] S6. Repeated operation can achieve sequential intermittent feeding of materials into the body;
[0013] S7, sodium hypophosphite and diisobutylene are mixed in the bulk. At this time, di-tert-butyl peroxide is introduced into the bulk and heated to generate sodium hypophosphite.
[0014] S8. The prepared sodium hypophosphite is then mixed with hydrogen chloride to react and generate dialkyl hypophosphite and sodium chloride.
[0015] S9, then after washing with water and extraction, dialkyl hypophosphoric acid can be obtained.
[0016] An apparatus for preparing dialkyl hypophosphoric acid, used to implement the preparation method of dialkyl hypophosphoric acid described in the above scheme, includes a body, wherein the body is provided with:
[0017] The feed inlet is used to communicate with the reaction chamber opened inside the main body;
[0018] Multiple feed blocks are used to transport raw materials;
[0019] Multiple feeding blocks move along predetermined paths and sequentially face the discharge port, so that various raw materials are intermittently fed into the reaction chamber through the discharge port in sequence.
[0020] Preferably, the feed block also includes a drive disk with a guide groove, and the feed block is provided with a guide block extending into the guide groove. The drive disk rotates to move the plurality of feed blocks.
[0021] Preferably, the guide groove includes a first annular groove and two second annular grooves, and the number of the feeding blocks is two. The drive disk rotates to make one of the guide blocks move along the first annular groove and the other guide block move along the second annular groove.
[0022] Preferably, the feeding block has a feed inlet on its side, and the main body has a feeding chamber that communicates with the feeding pipe. The notch on the feeding chamber is adapted to the feed inlet, and the inside of the feeding chamber is provided with a ramp for guiding the movement of raw materials.
[0023] Preferably, a fixing plate is also included, which is fixedly installed between the two feeding chambers to block the feed inlet.
[0024] Preferably, the feeding block is internally equipped with an extrusion plate;
[0025] When the feeding block is facing the discharge port, the extrusion plate moves down to force the raw materials and gas inside the feeding block into the reaction chamber.
[0026] Preferably, the feeding block is movably provided with gears and locking blocks. When the feeding block moves away from the discharge port, the gears rotate to drive the extrusion plate to a higher position and then be locked by the locking blocks.
[0027] Preferably, the device also includes a sealing plate for closing the discharge port, the sealing plate being rotated to open and close the discharge port.
[0028] Preferably, the sealing plate is provided with a push rod, the locking block is provided with a lever, the feeding block moves toward the discharge port so that the lever moves the push rod and opens the discharge port, and the push rod moves the lever to unlock the extrusion plate.
[0029] In the above technical solution, the preparation method and preparation equipment of dialkyl hypophosphite provided by the present invention have the following beneficial effects: it can realize small-scale and multiple reactions, avoid the violent reaction caused by mixing a large amount of raw materials, sodium hypophosphite and diisobutylene enter two cavities through two channels respectively, the drive disk rotates to drive the two cavities to move respectively, and feed the raw materials into the body in sequence for reaction, and during the feeding process, the extrusion plate in the cavity will move downward and press the gas in the cavity into the body to prevent the gas in the body from escaping. Attached Figure Description
[0030] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.
[0031] Figure 1 This is a schematic diagram of the overall structure provided in an embodiment of the present invention;
[0032] Figure 2 This is a schematic diagram of the structure of the reaction chamber provided in an embodiment of the present invention;
[0033] Figure 3 for Figure 2 Enlarged view of point A in the middle;
[0034] Figure 4This is a schematic diagram of the structure of the feeding block provided in an embodiment of the present invention;
[0035] Figure 5 for Figure 4 Enlarged view at point B in the middle;
[0036] Figure 6 This is a schematic diagram of the internal structure of the feeding block provided in an embodiment of the present invention;
[0037] Figure 7 for Figure 6 Enlarged view at point C;
[0038] Figure 8 This is a schematic diagram of the structure of the sealing plate provided in an embodiment of the present invention;
[0039] Figure 9 for Figure 8 Enlarged view at point D;
[0040] Figure 10 This is a schematic diagram of the drive disk provided in an embodiment of the present invention.
[0041] Explanation of reference numerals in the attached figures:
[0042] 1. Body; 11. Feeding block; 111. Extrusion plate; 112. First spring; 113. Gear; 114. Take-up reel; 115. First pull rope; 116. Locking block; 117. Lever; 118. Second spring; 119. Guide block; 12. Feeding pipe; 121. Feeding chamber; 122. Baffle; 123. Third spring; 124. Rack; 125. Fixing plate; 13. Discharge port; 131. Sealing plate ; 132. Push rod; 133. Torsion spring; 134. Shaft; 135. Chain; 14. Reaction chamber; 141. Storage chamber; 142. Guide ramp; 143. Divider block; 144. Movable rod; 145. Rocker arm; 146. Fourth spring; 147. Second pull rope; 15. Motor; 151. Drive disc; 152. Guide groove; 153. Paddle; 154. First annular groove; 155. Second annular groove. Implementation
[0043] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.
[0044] like Figures 1-10 As shown, a method for preparing dialkyl hypophosphoric acid includes the following steps:
[0045] S1, sodium hypophosphite, and diisobutylene enter the two cavities through two channels, respectively;
[0046] S2. The drive disk 151 is driven to rotate, thereby moving one of the cavities and gradually facing the feed port 13. The feed port 13 opens, allowing the raw material inside the cavity to enter the body 1.
[0047] S3. The extrusion plate 111 inside the cavity moves downward and forces the air that has escaped from the body 1 back into the body 1.
[0048] S4. Drive disk 151 is driven to rotate in the opposite direction so that the cavity returns to its initial position and the other cavity gradually faces the material below the feed port 13.
[0049] S5. When the cavity moves to the initial position, the extrusion plate 111 is driven to move upward, opening the cavity;
[0050] S6. Repeating the operation will allow for sequential intermittent feeding of materials into body 1;
[0051] S7, sodium hypophosphite and diisobutylene are mixed in bulk 1. At this time, di-tert-butyl peroxide is introduced into bulk 1 and heated to generate sodium hypophosphite.
[0052] S8. The prepared sodium hypophosphite is then mixed with hydrogen chloride to react and generate dialkyl hypophosphite and sodium chloride.
[0053] S9, then after washing with water and extraction, dialkyl hypophosphoric acid can be obtained.
[0054] Specifically, in the preparation of dialkyl hypophosphite using sodium hypophosphite and diisobutylene, a small amount of sodium hypophosphite and diisobutylene are added to the reaction vessel and heated. After reacting for a period of time, the reaction vessel needs to be opened and the raw materials added again. This is existing technology and will not be elaborated further.
[0055] Furthermore, sodium hypophosphite and diisobutylene are respectively introduced into two feeding pipes 12 and into two feeding chambers 121. The two raw materials enter the cavities inside the two feeding blocks 11 along the slope inside the feeding chamber 121. The drive disc 151 is driven to rotate clockwise, which in turn drives one of the feeding blocks 11 to move. The feeding block 11 gradually faces the discharge port 13. At this time, the lever 117 on the feeding block 11 moves the push rod 132 on the sealing plate 131, causing the sealing plate 131 to rotate, so that the raw materials inside the feeding block 11 enter the body 1. At the same time, the extrusion plate 11... 1. Moving downwards, the air escaping from body 1 is forced back into body 1; the drive disc 151 is driven to rotate counterclockwise, causing the feeding block 11 to gradually shift away from the discharge port 13, and the sealing plate 131 re-closes the discharge port 13. During the movement, the gear 113 rotates, causing the extrusion plate 111 to move upwards, and the feeding block 11 gradually returns to its initial position; the drive disc 151 continues to rotate counterclockwise, causing another feeding block 11 to move closer to the discharge port 13 and feed another raw material into the body 1; repeating the operation can realize the sequential intermittent feeding of materials into body 1.
[0056] Furthermore, in the above embodiments, the body 1 is specifically a microchannel reactor.
[0057] In the above technical solution, the main body 1 is used as a reaction vessel, which can realize small-scale and multiple reactions, avoiding the violent reaction caused by mixing a large amount of raw materials. Sodium hypophosphite and diisobutylene enter the two cavities through two channels respectively. The drive disk 151 rotates and drives the two cavities to move respectively, and feeds the raw materials into the main body 1 in sequence for reaction. During the feeding process, the extrusion plate 111 in the cavity will move downward and press the gas in the cavity into the main body 1, preventing the gas in the main body 1 from escaping.
[0058] As a further embodiment of the present invention, it includes a body 1, on which:
[0059] The discharge port 13 is used to communicate with the reaction chamber 14 opened inside the main body 1;
[0060] Multiple feeding blocks 11 are used to transport raw materials;
[0061] Multiple feeding blocks 11 move along predetermined paths and face the discharge port 13 in sequence, so that multiple raw materials are intermittently fed into the reaction chamber 14 through the discharge port 13 in sequence.
[0062] Specifically, the main body 1 has a chute for guiding the movement of the feeding block 11, the feeding block 11 has a cavity for storing raw materials, and the bottom of the cavity has a notch.
[0063] Furthermore, during the feeding process, multiple raw materials are first sent to the cavities on multiple feeding blocks 11, and then the multiple feeding blocks 11 are driven to move along a predetermined path. The notches at the bottom of the multiple feeding blocks 11 are aligned with the discharge port 13 on the main body 1, and the multiple raw materials inside the multiple feeding blocks 11 are sequentially fed into the reaction chamber 14 inside the main body 1 for reaction.
[0064] Furthermore, in the above embodiments, an electric telescopic rod can be provided between the feeding block 11 and the body 1. When material needs to be fed into the body 1, the electric telescopic rod extends, pushing the feeding block 11 closer to the lower feed port 13 to feed the raw material into the body 1. Alternatively, a motor can be provided on the body 1, with a pull rope between the motor's output end and the feeding block 11, and a spring between the feeding block 11 and the body 1. When material needs to be fed into the body 1, the motor operates to wind up the pull rope, pulling the feeding block 11 closer to the lower feed port 13 to feed the raw material into the body 1. The motor then stops working, and the spring pulls the feeding block 11 back to its initial position. Other structures that can be obtained by those skilled in the art based on common technical knowledge are also acceptable.
[0065] As a further embodiment of the present invention, it also includes a drive disk 151, on which a guide groove 152 is provided, and a guide block 119 extending into the guide groove 152 is provided on the feeding block 11. The drive disk 151 rotates to move the plurality of feeding blocks 11.
[0066] Specifically, a motor 15 is provided on the main body 1, and a drive disk 151 is provided on the output end of the motor 15.
[0067] Furthermore, during the feeding process, multiple raw materials are first fed into the cavities of multiple feeding blocks 11. At this time, the motor 15 drives the drive disk 151 to rotate. The guide groove 152 on the drive disk 151 pushes the guide block 119 on the feeding block 11, causing the multiple feeding blocks 11 to move along the slide groove on the body 1. The notches at the bottom of the multiple feeding blocks 11 are aligned with the discharge port 13 on the body 1. The multiple raw materials inside the multiple feeding blocks 11 are sequentially fed into the reaction chamber 14 inside the body 1 for reaction.
[0068] Furthermore, in the above embodiment, a series of circumferentially arrayed grooves can be formed on the main body 1. When the drive disk 151 rotates, the guide groove 152 drives the feeding block 11 to move along the groove on the main body 1, gradually moving from one end of the groove to the other end, and passing through the discharge port 13 to perform the feeding operation. After all the feeding blocks 11 have completed the feeding operation, the drive disk 151 can be rotated in the opposite direction to send the multiple feeding blocks 11 back to the initial position. Alternatively, other structures that can be obtained by those skilled in the art based on common technical knowledge can also be used.
[0069] As another embodiment of the present invention, the guide groove 152 includes a first annular groove 154 and two second annular grooves 155. The number of feeding blocks 11 is two. The drive disk 151 rotates so that one of the guide blocks 119 moves along the first annular groove 154 and the other guide block 119 moves along the second annular groove 155.
[0070] Specifically, a lever 153 is provided between the two second annular grooves 155.
[0071] Furthermore, during the feeding process, various raw materials are first fed into the cavities of multiple feeding blocks 11. At this time, the motor 15 drives the drive disk 151 to rotate. The second annular groove 155 on the drive disk 151 pushes the guide block 119 on one of the feeding blocks 11, causing the feeding block 11 to move along the slide groove on the body 1. The notch at the bottom of the feeding block 11 gradually aligns with the discharge port 13 on the body 1 to complete the feeding process. The guide block 119 on the feeding block 11 pushes against the paddle 153, causing the paddle 153 to move the other feeding block 11. One second annular groove 155 is blocked to prevent the guide block 119 from entering another second annular groove 155, while the guide block 119 on the other feeding block 11 moves along the first annular groove 154, and the feeding block 11 does not move. Then the motor 15 drives the drive disk 151 to rotate in the opposite direction so that the feeding block 11 that completes the feeding work is gradually returned to its original position, while the other feeding block 11 is pushed to move and complete the feeding work. The two raw materials inside the two feeding blocks 11 are sequentially put into the reaction chamber 14 inside the body 1 to react.
[0072] As another embodiment of the present invention, the feeding block 11 has a feeding port on its side, and the body 1 has a feeding cavity 121 that communicates with the feeding pipe 12. The notch on the feeding cavity 121 is adapted to the feeding port, and the inside of the feeding cavity 121 is provided with a ramp for guiding the movement of raw materials.
[0073] Specifically, a baffle 122 is movably provided on the main body 1 to block the notch on the feeding chamber 121, and a third spring 123 is provided between the baffle 122 and the main body 1.
[0074] Furthermore, when the feeding block 11 is in its initial position, the feed inlet on the side of the feeding block 11 is directly opposite the notch on the feeding chamber 121. At this time, the feeding pipe 12 passes through the raw material and slides into the cavity inside the feeding block 11 along the slope inside the feeding chamber 121. At this time, the drive disc 151 rotates, causing the feeding block 11 to move closer to the lower feed port 13. At this time, the third spring 123 pushes against the baffle 122, and the baffle 122 seals the notch on the feeding chamber 121 to prevent the raw material from leaking. After the feeding block 11 completes the feeding work, it gradually moves closer to the feeding chamber 121 and pushes against the baffle 122, so that the baffle 122 returns to the body 1, so that the feeding chamber 121 can feed the feeding block 11.
[0075] As another embodiment of the present invention, a fixing plate 125 is also included, which is fixedly installed between the two feeding chambers 121 to block the feed inlet.
[0076] Specifically, the fixing plate 125 cooperates with the feeding block 11 to block the feed inlet on the side of the feeding block 11. When the feeding block 11 finishes feeding and approaches the lower feed port 13, the fixing plate 125 seals the feed inlet on the side of the feeding block 11 to prevent raw material leakage.
[0077] As another embodiment of the present invention, a pressing plate 111 is movably disposed inside the feeding block 11;
[0078] When the feeding block 11 is facing the discharge port 13, the extrusion plate 111 moves down to force the raw materials and gas inside the feeding block 11 into the reaction chamber 14.
[0079] Specifically, during the feeding process, the feeding block 11 moves closer to the lower feed port 13. When the feeding block 11 is directly facing the lower feed port 13, the lower feed port 13 opens, and the raw material in the feeding block 11 falls into the body 1. At the same time, the gas in the body 1 enters the cavity of the feeding block 11. At this time, the extrusion plate 111 is driven to move downward, pressing the remaining raw material and gas inside the feeding block 11 into the body 1 together, preventing gas leakage from the body 1. After the feeding process is completed, the feeding block 11 moves closer to the upper feed chamber 121. At this time, the lower feed port 13 closes, and the extrusion plate 111 moves upward, leaving a cavity inside the feeding block 11 for storing raw materials.
[0080] Furthermore, in the above embodiments, an electric telescopic rod may be provided between the feeding block 11 and the extrusion plate 111. During the unloading operation, the electric telescopic rod extends, pushing the extrusion plate 111 downward. After the unloading operation is completed, the electric telescopic rod shortens, driving the extrusion plate 111 upward. Alternatively, a motor may be provided inside the feeding block 11, with a pull rope between the motor's output end and the extrusion plate 111, and a spring between the extrusion plate 111 and the feeding block 11. During the unloading operation, the motor operates, releasing the rope, and the spring pushes the extrusion plate 111 downward. After the unloading operation is completed, the motor operates, winding up the pull rope, driving the extrusion plate 111 upward. Other structures that can be obtained by those skilled in the art based on common technical knowledge are also acceptable.
[0081] As another embodiment of the present invention, a gear 113 and a locking block 116 are movably provided on the feeding block 11. When the feeding block 11 moves away from the discharge port 13, the gear 113 rotates to drive the extrusion plate 111 to move up to a high position and then is locked by the locking block 116.
[0082] Specifically, the main body 1 is symmetrically provided with racks 124 that mesh with gears 113. A take-up reel 114 is movably provided on gears 113. A ratchet and pawl mechanism is provided between gears 113 and take-up reel 114. A first pull rope 115 is provided between take-up reel 114 and extrusion plate 111. A first spring 112 is provided between extrusion plate 111 and feeding block 11. A second spring 118 is provided between locking block 116 and feeding block 11. A ramp is provided at the bottom of locking block 116.
[0083] Furthermore, as the feeding block 11 moves away from the discharge port 13, the gear 113 on the feeding block 11 gradually meshes with the rack 124. The movement of the feeding block 11 drives the gear 113 to rotate, which in turn drives the take-up reel 114 to rotate and wind up the first pull rope 115. This pulls the extrusion plate 111 upwards and along the slope at the bottom of the locking block 116, pushing the locking block 116 into the feeding block 11. After the extrusion plate 111 separates from the locking block 116, the locking block... 116 extends under the action of the second spring 118 and supports the extrusion plate 111; when the feeding block 11 moves toward the discharge port 13, the gear 113 rotates but cannot transmit force to the take-up reel 114. When the feeding block 11 is facing the discharge port 13, the discharge port 13 opens, the locking block 116 is driven to move and retract into the feeding block 11, and the extrusion plate 111 moves downward under the push of the first spring 112, pressing the raw material and gas inside the feeding block 11 into the body 1.
[0084] As another embodiment of the present invention, it also includes a sealing plate 131 for closing the discharge port 13, the sealing plate 131 being rotated to open and close the discharge port 13.
[0085] Specifically, during the feeding process, when the feeding block 11 is facing the feeding port 13, the sealing plate 131 is driven to rotate, opening the feeding port 13. The raw material inside the feeding block 11 passes through the feeding port 13 and enters the body 1 under the action of gravity, so as to carry out the reaction. After the feeding process is completed, the feeding block 11 separates from the feeding port 13. At this time, the sealing plate 131 rotates to reseal the feeding port 13.
[0086] As another embodiment of the present invention, a push rod 132 is provided on the sealing plate 131, and a lever 117 is provided on the locking block 116. The feeding block 11 moves to the lower feed port 13 so that the lever 117 moves the push rod 132 and opens the feed port 13. The push rod 132 moves the lever 117 to unlock the extrusion plate 111.
[0087] Specifically, a shaft 134 is provided on the sealing plate 131, an "8"-shaped chain 135 is provided between the two shafts 134 on the sealing plate 131, and a torsion spring 133 is provided between the shaft 134 and the body 1.
[0088] Furthermore, as the feeding block 11 moves away from the discharge port 13, the gear 113 on the feeding block 11 gradually meshes with the rack 124. The movement of the feeding block 11 drives the gear 113 to rotate, which in turn drives the take-up reel 114 to rotate and wind up the first pull rope 115. This pulls the extrusion plate 111 upwards and along the slope at the bottom of the locking block 116, pushing the locking block 116 into the feeding block 11. After the extrusion plate 111 separates from the locking block 116, the locking block 116 extends under the action of the second spring 118 and supports the extrusion plate 111. As the feeding block 11 moves closer to the discharge port... When the direction of 13 moves, gear 113 rotates but cannot transmit force to take-up reel 114. As the feeding block 11 gradually faces the discharge port 13, lever 117 pushes push rod 132, causing sealing plate 131 to rotate against the resistance of torsion spring 133. Sealing plate 131 drives another sealing plate 131 to rotate through chain 135, opening discharge port 13. Lever 117 drives locking block 116 to move, locking block 116 retracts into the feeding block 11. Extrusion plate 111 moves downward under the push of first spring 112, forcing the raw material and gas inside feeding block 11 into body 1.
[0089] As a further embodiment of the present invention, the reaction chamber 14 is provided with a symmetrical guide ramp 142 inside, the highest point of the guide ramp 142 is directly opposite the center of the discharge port 13, the reaction chamber 14 is provided with a symmetrical storage chamber 141 inside, the storage chamber 141 is located below the guide ramp 142, the reaction chamber 14 is provided with a notch to facilitate the raw material to fall into the storage chamber 141 along the guide ramp 142, the body 1 is symmetrically and movably provided with a material distribution block 143, the material distribution block 143 is slidably provided on the guide ramp 142, the body 1 is movably provided with a movable rod 144 inside, the movable rod 144 and the two material distribution blocks 143 are movably provided with rocker arms 145, the movable rod 144 and the body 1 are provided with a fourth spring 146, and the movable rod 144 and the drive disc 151 are provided with a second pull rope 147.
[0090] Specifically, during the feeding operation, the feeding block 11 is in its initial position, with the feed inlet on the side of the feeding block 11 aligned with the notch on the feeding chamber 121. At this time, the raw material is fed through the feeding pipe 12 and slides along the slope inside the feeding chamber 121 into the cavity inside the feeding block 11. Simultaneously, the motor 15 drives the drive disc 151 to rotate, and the second annular groove 155 on the drive disc 151 pushes the guide block 119 on one of the feeding blocks 11, causing the feeding block 11 to move along the sliding groove on the body 1. The baffle 122 moves under the action of the third spring 123 and seals the feeding chamber 121. This feeding... The notch at the bottom of block 11 gradually aligns with the discharge port 13 on the main body 1 to complete the feeding operation. The guide block 119 on the feeding block 11 pushes against the paddle 153, causing the paddle 153 to block another second annular groove 155, preventing the guide block 119 from entering the other second annular groove 155. Meanwhile, the guide block 119 on the other feeding block 11 moves along the first annular groove 154, while the corresponding feeding block 11 does not move. When the drive disc 151 rotates, it will wind up the second pull rope 147, causing the movable rod 144 to move upward, driving the material distribution block 143 to move upward along the guide slope 142 and gradually approach each other.
[0091] As the feeding block 11 moves toward the discharge port 13, the gear 113 rotates but cannot transmit force to the take-up reel 114. As the feeding block 11 gradually faces the discharge port 13, the lever 117 pushes the push rod 132, causing the sealing plate 131 to rotate against the resistance of the torsion spring 133. The sealing plate 131 drives another sealing plate 131 to rotate through the chain 135, opening the discharge port 13. The lever 117 drives the locking block 116 to move, and the locking block 116 retracts into the feeding block 11. The extrusion plate 111 moves downward under the push of the first spring 112, pressing the raw materials and gas inside the feeding block 11 into the body 1.
[0092] The raw material falls into the reaction chamber 14 through the feed inlet 13, first landing on two dividing blocks 143 and being divided into two roughly equal portions. These portions then move downwards along the guide ramp 142 into the storage chamber 141. At this time, the drive disc 151 rotates in the opposite direction, causing the feeding block 11 to move away from the feed inlet 13. The lever 117 separates from the push rod 132. The sealing plate 131, under the action of the torsion spring 133, seals the feed inlet 13. Meanwhile, the gear 113 on the feeding block 11 gradually meshes with the rack 124. As the feeding block 11 moves, it drives the gear 113 to rotate. The gear 113 drives the take-up reel 114 to rotate, winding up the first pull rope 115 and pulling the extrusion plate 111 upwards along the locking block. The slope at the bottom of 116 moves, pushing the locking block 116 to retract into the feeding block 11. After the extrusion plate 111 separates from the locking block 116, the locking block 116 extends under the action of the second spring 118 and supports the extrusion plate 111. While the drive disc 151 rotates, it will gradually loosen the second pull rope 147. The fourth spring 146 pushes the movable rod 144 downward and pushes the material distribution block 143 to move through the rocker arm 145. The material distribution block 143 moves along the guide slope 142, pushing the residual material on the guide slope 142 into the storage chamber 141 for reaction. When it reaches the lowest point, it seals the gap on the reaction chamber 14 to prevent the gas or liquid generated by the violent reaction from moving upward from the gap on the reaction chamber 14.
[0093] The drive disk 151 continues to rotate, driving the feeding block 11 to move closer to the upper material cavity 121 and push the baffle 122 to retract into the body 1. The feeding block 11 is directly facing the upper material cavity 121. The drive disk 151 continues to rotate, driving another feeding block 11 to perform feeding work. Repeated operation can realize the sequential intermittent feeding of two materials, which is safe and convenient.
[0094] The foregoing has only described certain exemplary embodiments of the present invention by way of illustration. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the foregoing drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.
Claims
1. An apparatus for preparing dialkyl hypophosphoric acid, characterized in that, Includes a body, on which are provided: The feed inlet is used to communicate with the reaction chamber opened inside the main body; Multiple feed blocks are used to transport raw materials; Multiple feeding blocks move along predetermined paths and sequentially face the discharge port, so that multiple raw materials are intermittently fed into the reaction chamber through the discharge port in sequence. It also includes a drive disk, on which a guide groove is provided, and on the feeding block a guide block extending into the guide groove is provided, and the drive disk rotates to move the plurality of feeding blocks; The guide groove includes a first annular groove and two second annular grooves. The number of the feeding blocks is two. The drive disk rotates to make one of the guide blocks move along the first annular groove and the other guide block move along the second annular groove. A paddle is provided between the two second annular grooves. An extrusion plate is movably arranged inside the feeding block; When the feeding block is facing the discharge port, the extrusion plate moves down to force the raw materials and gas inside the feeding block into the reaction chamber.
2. The apparatus for preparing dialkyl hypophosphoric acid according to claim 1, characterized in that, The feeding block has a feed inlet on its side, and the main body has a feeding chamber that communicates with the feeding pipe. The notch on the feeding chamber is adapted to the feed inlet, and the inside of the feeding chamber is provided with a ramp for guiding the movement of raw materials.
3. The apparatus for preparing dialkyl hypophosphoric acid according to claim 2, characterized in that, It also includes a fixing plate, which is fixedly installed between the two feeding chambers to block the feed inlet.
4. The apparatus for preparing dialkyl hypophosphoric acid according to claim 3, characterized in that, The feeding block is movably equipped with gears and locking blocks. When the feeding block moves away from the discharge port, the gears rotate to drive the extrusion plate to a higher position, where it is then locked by the locking blocks.
5. The apparatus for preparing dialkyl hypophosphoric acid according to claim 4, characterized in that, It also includes a sealing plate for closing the discharge port, the sealing plate being rotated to open and close the discharge port.
6. The apparatus for preparing dialkyl hypophosphoric acid according to claim 5, characterized in that, The sealing plate is provided with a push rod, and the locking block is provided with a lever. The feeding block moves toward the discharge port so that the lever moves the push rod and opens the discharge port. The push rod moves the lever to unlock the extrusion plate.
Citation Information
Patent Citations
Method for synthesizing bis(2,4,4-trimethylpentyl) phosphinic acid with double initiators
CN102268038A
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