Intermediate preparation device for rubber production

Abstract

The utility model discloses an intermediate preparation device for rubber production, and relates to the technical field of biphenyl sulfonation reaction, the intermediate preparation device comprises a rack, a reaction box fixedly connected to the top end of the rack, a feeding mechanism used for adjusting the flow rate of materials entering an inner cavity of the reaction box, and a transfer pipe fixedly connected to the outer surface of the feeding mechanism, by arranging the feeding mechanism, materials entering the inner cavity of the transfer pipe can be blocked, and the speed of the materials entering the inner cavity of the transfer pipe can be changed under the control of an operator, so that when the materials in the inner cavity of the reaction box react, the materials in the inner cavity of the reaction box can be separated from the inner cavity of the reaction box. The top of the transfer pipe is closed; and by arranging the stirring mechanism, materials entering the inner cavity of the reaction box can be stirred, so that the materials can fully react, and the effect of preventing waste gas leakage in the reaction process is achieved.

Description

Technical Field

[0001] This invention relates to the field of biphenyl sulfonation reaction technology, specifically to an apparatus for preparing intermediates for rubber production. Background Technology

[0002] 4-Hydroxybiphenyl is an intermediate material in rubber manufacturing. Biphenyl sulfonation is a chemical reaction that introduces a sulfonic acid group into the biphenyl molecule. The following is a formal description of the biphenyl sulfonation reaction: Biphenyl sulfonation typically uses concentrated sulfuric acid or fuming sulfuric acid as the sulfonating agent. In the reaction, the sulfonating agent undergoes an electrophilic substitution reaction with biphenyl, where the sulfonic acid group replaces a hydrogen atom in the biphenyl molecule, generating biphenyl sulfonic acid. The specific steps of the reaction are as follows: Preparation of reactants: Biphenyl and the sulfonating agent are added to a reaction vessel in a specific ratio. Heating the reaction: The reaction mixture is heated at an appropriate temperature to allow the sulfonation reaction to proceed. The reaction temperature and time affect the yield and the properties of the product. Reaction monitoring: The degree of completion of the reaction is determined by monitoring the reaction progress. Chemical analysis methods, such as thin-layer chromatography (TLC) or high-performance liquid chromatography (HPLC), can be used to monitor the reaction. Post-processing: After the reaction is complete, the reaction mixture is post-processed, such as neutralized, filtered, and washed, to obtain the sulfonated product.

[0003] The conditions of sulfonation reactions (such as reaction temperature, reaction time, and amount of sulfonating agent) affect the reaction yield and the properties of the product. Safety precautions must be taken during sulfonation reactions to avoid leakage and contact with the sulfonating agent. Furthermore, depending on the specific reaction requirements and the intended use of the product, further purification and processing of the sulfonated product may be necessary.

[0004] When preparing intermediates for rubber production, various materials need to be poured into test tubes for reaction; however, in commercially available products, after the materials are poured into a reactor vessel, the waste gas generated during the reaction may leak due to the vessel's opening. Summary of the Invention

[0005] To achieve the above objectives, the present invention provides the following technical solution: an apparatus for preparing intermediates for rubber production, comprising a frame and a reaction chamber fixedly connected to the top of the frame.

[0006] The feeding mechanism is used to regulate the flow rate of the material entering the inner cavity of the reaction chamber, and a transfer pipe is fixedly connected to the outer surface of the feeding mechanism. The bottom end of the transfer pipe is fixedly connected to a connecting pipe. By setting the feeding mechanism, the material entering the inner cavity of the transfer pipe can be blocked, and the speed at which the material enters the inner cavity of the transfer pipe can be changed under the control of the operator, so as to achieve the effect that the top of the transfer pipe is closed when the material reacts in the inner cavity of the reaction chamber.

[0007] The stirring mechanism is used to agitate the materials entering the reaction chamber, thereby enabling the materials to react fully and accelerating the reaction rate. The stirring mechanism is used to mix the solution in the reaction chamber.

[0008] The connecting pipe is fixedly connected to the upper surface of the reaction chamber and penetrates through the reaction chamber; the stirring mechanism is fixedly connected to the inner cavity of the reaction chamber.

[0009] The feeding mechanism includes a fixed tube, which is fixedly connected to the top of the transfer tube. A partition is fixedly connected to the bottom of the fixed tube. There are several partitions, which are evenly distributed. A bottom frame is fixedly connected to the bottom of each partition. By setting the fixed tube and partitions, many gaps can be generated, so that the solution required for the reaction can leak into the inner cavity of the transfer tube through the gaps.

[0010] Preferably, a funnel is slidably connected to the inner cavity of the fixed tube, a handle is fixedly connected to the outer surface of the funnel, and a partition rod is fixedly connected to the bottom end of the funnel. The number of partition rods is several, and the partition rods are evenly distributed. By setting the funnel, it is convenient for the operator to pour the materials required for the experiment into the inner cavity of the transfer tube. By setting the partition rod, the materials can flow out through the bottom end of the funnel and flow into the gap formed by the partition.

[0011] Preferably, a blocking block is fixedly connected to the bottom end of the partition rod, and a sealing ring is fixedly connected to the outer surface of the blocking block. The sealing ring is rubbed and adapted to the inner surface of the partition. By setting the blocking block and the sealing ring, the gap formed by several partitions can be blocked, thereby preventing the solution from leaking out from the bottom end of the funnel.

[0012] Preferably, a spring is fixedly connected to the side of the lower surface of the blocking block. The number of springs is several and they are evenly distributed. The springs are pressed and adapted to the bottom surface of the inner cavity of the bottom frame. A spring is fixedly connected to the lower surface of the blocking block. The bottom end of the spring is fixedly connected to the bottom surface of the inner cavity of the bottom frame. By setting the spring and the spring, the blocking block can rebound after it moves downward and when the operator does not press the funnel.

[0013] Preferably, the stirring mechanism includes a fixed plate, which is fixedly connected to the bottom of the inner wall of the reaction tank. A drain pipe extends through the side of the lower surface of the fixed plate, and a blocking rod is provided on the inner wall of the drain pipe. By providing the drain pipe, the solution on the upper surface of the fixed plate can be discharged, and by providing the blocking rod, the drain pipe can be blocked.

[0014] Preferably, a fixing rod is fixedly connected to the lower surface of the fixing disk, and a servo motor is fixedly connected to the end of the fixing rod. A rotating rod is installed at the output end of the servo motor through a coupling. The rotating rod passes through the fixing disk. By setting the servo motor, the rotating rod can be made to rotate after the power is connected and the switch is turned on.

[0015] Preferably, a mixing disk is fixedly connected to the top end of the rotating rod, and the stirring mechanism further includes a connecting frame. The connecting frame is fixedly connected to the inner wall of the reaction tank, and a fixing block is fixedly connected to the end of the connecting frame. A stirring plate is fixedly connected to the lower surface of the fixing block. The stirring plate is located in the inner cavity of the mixing disk. By setting the stirring plate, it can rotate relative to the mixing disk when the mixing disk rotates, thereby stirring the solution in the inner cavity of the mixing disk. A support rod is fixedly connected to the outer surface of the rotating rod, and a scraper is fixedly connected to the bottom end of the support rod. A scraper blade is fixedly connected to the lower surface of the scraper. The scraper blade is rubbed and adapted to the upper surface of the fixed disk. By setting the scraper blade and scraper, the material on the upper surface of the fixed disk can be stirred during the rotation of the rotating rod.

[0016] A process for preparing an intermediate for rubber production includes the following steps:

[0017] Step 1: Sulfuric acid and biphenyl are poured into two separate feed mechanisms, and then enter the inner cavity of the reaction chamber to undergo sulfonation, thus preparing biphenyl-4-sulfonic acid;

[0018] Step 2: Pour the neutralization solution into the inner cavity of the reaction chamber and neutralize the biphenyl-4-sulfonic acid to obtain the corresponding sulfonate.

[0019] Step 3: Heat the outer wall of the reaction chamber and control the temperature at 290-340℃. Use an aqueous solution of alkali metal hydroxide with a concentration of 50%-96% by weight to perform alkaline pressure hydrolysis of biphenyl-4-sulfonic acid under a pressure not exceeding 120 bar. The molar ratio of alkali metal hydroxide to alkali metal salt of biphenyl sulfonic acid is 3-25:1.

[0020] Step 4: Dilute the alkaline reaction mixture with water and acidify it with an inorganic acid to a pH value of 0 to less than 6.5. Then heat the acidified reaction mixture at a temperature above 115°C and a pH value of less than 6.5 for 5 minutes to 5 hours to obtain 4-hydroxybiphenyl.

[0021] This invention provides an apparatus for preparing intermediates for rubber production. It has the following advantages:

[0022] I. This intermediate preparation device for rubber production, by setting up a feeding mechanism, can block the material entering the inner cavity of the transfer tube, and under the control of the operator, the speed at which the material enters the inner cavity of the transfer tube can be changed, thereby achieving the effect that the top of the transfer tube is closed when the material reacts in the inner cavity of the reaction chamber.

[0023] II. The intermediate preparation device for rubber production, by setting up a stirring mechanism, can stir the materials entering the inner cavity of the reaction chamber, thereby enabling the materials to react fully and accelerating the reaction speed.

[0024] III. This intermediate preparation device for rubber production, by setting a funnel, allows operators to easily pour the materials required for the experiment into the inner cavity of the transfer tube. By setting a partition rod, the material can flow out through the bottom of the funnel and into the gap formed by the partitions. By setting a blocking block and a sealing ring, the gap formed by several partitions can be blocked, thereby preventing the solution from leaking out from the bottom of the funnel. By setting a spring and a spring, the blocking block can rebound after it moves downward and when the operator does not press the funnel.

[0025] IV. This intermediate preparation device for rubber production can drain the solution from the surface of the fixed plate by setting a drain pipe, block the drain pipe by setting a blocking rod, rotate the rotating rod after the power is connected and the switch is turned on by setting a servo motor, rotate relative to the mixing plate when the mixing plate rotates, and stir the solution in the cavity of the mixing plate by setting a stirring plate, and stir the material on the surface of the fixed plate during the rotation of the rotating rod by setting scraper and scraper blade. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the external structure of an intermediate preparation apparatus for rubber production according to the present invention;

[0027] Figure 2 This is a cross-sectional structural schematic diagram of an intermediate preparation apparatus for rubber production according to the present invention;

[0028] Figure 3 This is a schematic diagram of the feeding mechanism of the present invention;

[0029] Figure 4 This is a partial structural diagram of the feeding mechanism of the present invention;

[0030] Figure 5 This is a schematic diagram of the stirring mechanism of the present invention;

[0031] Figure 6 This is a partial structural diagram of the stirring mechanism of the present invention;

[0032] Figure 7 This is a process flowchart for preparing an intermediate for rubber production according to the present invention.

[0033] In the diagram: 1. Frame; 2. Reaction chamber; 3. Connecting pipe; 4. Transfer pipe; 5. Feeding mechanism; 6. Stirring mechanism; 51. Fixed pipe; 52. Partition block; 53. Base frame; 54. Funnel; 55. Partition rod; 56. Blocking block; 57. Sealing ring; 58. Spring; 59. Spring; 510. Handle; 61. Fixed plate; 62. Fixed rod; 63. Servo motor; 64. Rotating rod; 65. Drain pipe; 66. Blocking rod; 67. Mixing plate; 68. Connecting frame; 69. Fixed block; 610. Stirring plate; 611. Support rod; 612. Scraper; 613. Scraper blade. Detailed Implementation

[0034] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention are given for illustrative and descriptive purposes only, and are not intended to be exhaustive or to limit the invention to the forms disclosed. Many modifications and variations will be apparent to those skilled in the art. The embodiments were chosen and described to better illustrate the principles and practical application of the invention, and to enable those skilled in the art to understand the invention and design various embodiments with various modifications suitable for a particular purpose.

[0035] First embodiment, such as Figures 1-4 As shown, the present invention provides a technical solution: an apparatus for preparing intermediates for rubber production, comprising a frame 1 and a reaction chamber 2 fixedly connected to the top of the frame 1.

[0036] The feeding mechanism 5 is used to adjust the flow rate of the material entering the inner cavity of the reaction chamber 2, and the transfer pipe 4 is fixedly connected to the outer surface of the feeding mechanism 5. The bottom end of the transfer pipe 4 is fixedly connected to the connecting pipe 3. By setting the feeding mechanism 5, the material entering the inner cavity of the transfer pipe 4 can be blocked, and the speed at which the material enters the inner cavity of the transfer pipe 4 can be changed under the control of the operator, so as to achieve the effect that the top of the transfer pipe 4 is closed when the material reacts in the inner cavity of the reaction chamber 2.

[0037] The stirring mechanism 6 is used to stir the material entering the inner cavity of the reaction tank 2, so that the material can react fully and the reaction speed can be accelerated. The stirring mechanism 6 is used to mix the solution in the inner cavity of the reaction tank 2.

[0038] The connecting pipe 3 is fixedly connected to the upper surface of the reaction chamber 2, and the connecting pipe 3 penetrates the reaction chamber 2. The stirring mechanism 6 is fixedly connected to the inner cavity of the reaction chamber 2.

[0039] The feeding mechanism 5 includes a fixed tube 51, which is fixedly connected to the top of the transfer tube 4. A partition 52 is fixedly connected to the bottom of the fixed tube 51. There are several partitions 52, which are evenly distributed. A bottom frame 53 is fixedly connected to the bottom of the partitions 52. By setting the fixed tube 51 and the partitions 52, many gaps can be generated, so that the solution required for the reaction can leak into the inner cavity of the transfer tube 4 through the gaps.

[0040] A funnel 54 is slidably connected to the inner cavity of the fixed tube 51. A handle 510 is fixedly connected to the outer surface of the funnel 54. A partition rod 55 is fixedly connected to the bottom end of the funnel 54. The partition rods 55 are evenly distributed. By setting the funnel 54, the operator can easily pour the materials needed for the experiment into the inner cavity of the transfer tube 4. By setting the partition rods 55, the materials can flow out through the bottom end of the funnel 54 and into the gap formed by the partition blocks 52. A blocking block 56 is fixedly connected to the bottom end of the partition rod 55. A sealing ring 57 is fixedly connected to the outer surface of the blocking block 56. The sealing ring 57 is rubbed and adapted to the inner surface of the partition block 52. By setting the blocking block 56 and the sealing ring 57, the gap formed by the partition blocks 52 can be blocked, thereby preventing the solution from leaking out from the bottom end of the funnel 54. A spring piece 5 is fixedly connected to the side of the lower surface of the blocking block 56. 8. The number of spring pieces 58 is several, and the several spring pieces 58 are evenly distributed. The several spring pieces 58 are pressed and adapted to the bottom surface of the inner cavity of the bottom frame 53. A spring 59 is fixedly connected to the lower surface of the blocking block 56. The bottom end of the spring 59 is fixedly connected to the bottom surface of the inner cavity of the bottom frame 53. By setting the spring pieces 58 and the spring 59, the blocking block 56 can rebound after it moves downward and when the operator does not press the funnel 54. In use, the operator pours the solution required for the reaction into the inner cavity of the funnel 54, then holds the handle 510 and pulls it down. During the pulling process, the blocking block 56 and the sealing ring 57 are separated from the space formed by the partition 52, so that the solution can leak into the inner cavity of the transfer tube 4. Then, the funnel 54 is released. Under the action of the spring pieces 58 and the spring 59, the blocking block 56 and the sealing ring 57 rebound, so that the gap between the partitions 52 is blocked.

[0041] Second embodiment, such as Figures 5-7As shown, the stirring mechanism 6 includes a fixed plate 61, which is fixedly connected to the bottom of the inner wall of the reaction tank 2. A drain pipe 65 passes through the side of the lower surface of the fixed plate 61, and a blocking rod 66 is provided on the inner wall of the drain pipe 65. The drain pipe 65 allows the solution on the upper surface of the fixed plate 61 to be drained, and the blocking rod 66 can block the drain pipe 65. A fixing rod 62 is fixedly connected to the lower surface of the fixed plate 61, and a servo motor 63 is fixedly connected to the end of the fixing rod 62. A rotating rod 64 is mounted on the output end of the servo motor 63 via a coupling. The rotating rod 64 passes through the fixed plate 61. By providing the servo motor 63, the rotating rod 64 can be rotated after the power is connected and the switch is turned on. A mixing plate 67 is fixedly connected to the top of the rotating rod 64. The stirring mechanism 6 also includes a connecting frame 68, which is fixedly connected to the inner wall of the reaction tank 2. A fixing block 69 is fixedly connected to the end of the connecting frame 68. A stirring plate 610 is fixedly connected to the lower surface of block 69. The stirring plate 610 is located in the inner cavity of the mixing disk 67. By setting the stirring plate 610, it can rotate relative to the mixing disk 67 when the mixing disk 67 rotates, thereby stirring the solution in the inner cavity of the mixing disk 67. A support rod 611 is fixedly connected to the outer surface of the rotating rod 64. A scraper 612 is fixedly connected to the bottom end of the support rod 611. A scraper blade 613 is fixedly connected to the lower surface of the scraper blade 612. The scraper 613 is frictionally adapted to the upper surface of the fixed disk 61. By setting the scraper 613 and scraper 612, the material on the upper surface of the fixed disk 61 can be stirred during the rotation of the rotating rod 64. In use, the operator connects the servo motor 63 to the power supply and turns on the switch of the servo motor 63, so that the rotating rod 64 drives the mixing disk 67 to rotate. The material will leak onto the upper surface of the mixing disk 67, and the stirring plate 610 will stir the material during the rotation, so that the solution is fully mixed.

[0042] A process for preparing an intermediate for rubber production includes the following steps:

[0043] Step 1: Sulfuric acid and biphenyl are poured into two feed mechanisms 5 respectively, and then enter the inner cavity of the reaction chamber 2 to obtain sulfonation and prepare biphenyl-4-sulfonic acid;

[0044] Step 2: Pour the neutralization solution into the inner cavity of reaction tank 2 and neutralize the biphenyl-4-sulfonic acid to obtain the corresponding sulfonate.

[0045] Step 3: Heat the outer wall of reaction chamber 2 and control the temperature at 290-340℃. Use an aqueous solution of alkali metal hydroxide with a concentration of 50%-96% by weight to perform alkaline pressure hydrolysis of biphenyl-4-sulfonic acid under a pressure not exceeding 120 bar. The molar ratio of alkali metal hydroxide to alkali metal salt of biphenyl sulfonic acid is 3-25:1.

[0046] Step 4: Dilute the alkaline reaction mixture with water and acidify it with an inorganic acid to a pH value of 0 to less than 6.5. Then heat the acidified reaction mixture at a temperature above 115°C and a pH value of less than 6.5 for 5 minutes to 5 hours to obtain 4-hydroxybiphenyl.

[0047] Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments obtained by those skilled in the art and related fields based on the embodiments of the present invention without inventive effort should fall within the scope of protection of the present invention. Structures, devices, and operating methods not specifically described and explained in the present invention, unless otherwise specified or limited, shall be implemented according to conventional means in the art.

Claims

1. An apparatus for preparing intermediates for rubber production, characterized in that, include: The frame (1) and the reaction chamber (2) fixedly connected to the top of the frame (1): Feeding mechanism (5), which is used to adjust the flow rate of the material entering the inner cavity of the reaction chamber (2), and transfer pipe (4) fixedly connected to the outer surface of the feeding mechanism (5), wherein the bottom end of the transfer pipe (4) is fixedly connected to a connecting pipe (3); A stirring mechanism (6) is used to mix the solution in the cavity of the reaction tank (2); The connecting pipe (3) is fixedly connected to the upper surface of the reaction tank (2), the connecting pipe (3) passes through the reaction tank (2), and the stirring mechanism (6) is fixedly connected to the inner cavity of the reaction tank (2); The feeding mechanism (5) includes a fixed tube (51), which is fixedly connected to the top of the transfer tube (4). A partition (52) is fixedly connected to the bottom of the fixed tube (51). There are several partitions (52), which are evenly distributed. A bottom frame (53) is fixedly connected to the bottom of the partitions (52).

2. The apparatus for preparing intermediates for rubber production according to claim 1, characterized in that: A funnel (54) is slidably connected to the inner cavity of the fixed tube (51). A handle (510) is fixedly connected to the outer surface of the funnel (54). A partition rod (55) is fixedly connected to the bottom end of the funnel (54). There are several partition rods (55), and the several partition rods (55) are evenly distributed.

3. The apparatus for preparing intermediates for rubber production according to claim 2, characterized in that: A blocking block (56) is fixedly connected to the bottom end of the partition rod (55), and a sealing ring (57) is fixedly connected to the outer surface of the blocking block (56). The sealing ring (57) is rubbed and adapted to the inner surface of the partition block (52).

4. The apparatus for preparing intermediates for rubber production according to claim 3, characterized in that: A spring (58) is fixedly connected to the side of the lower surface of the blocking block (56). There are several springs (58), and the several springs (58) are evenly distributed. The several springs (58) are pressed and adapted to the bottom surface of the inner cavity of the bottom frame (53). A spring (59) is fixedly connected to the lower surface of the blocking block (56), and the bottom end of the spring (59) is fixedly connected to the bottom surface of the inner cavity of the bottom frame (53).

5. The apparatus for preparing intermediates for rubber production according to claim 1, characterized in that: The stirring mechanism (6) includes a fixed plate (61), which is fixedly connected to the bottom of the inner wall of the reaction tank (2). A drain pipe (65) is passed through the side of the lower surface of the fixed plate (61), and a blocking rod (66) is provided on the inner wall of the drain pipe (65).

6. The apparatus for preparing intermediates for rubber production according to claim 5, characterized in that: A fixing rod (62) is fixedly connected to the lower surface of the fixing disk (61), and a servo motor (63) is fixedly connected to the end of the fixing rod (62). A rotating rod (64) is installed at the output end of the servo motor (63) through a coupling, and the rotating rod (64) passes through the fixing disk (61).

7. The apparatus for preparing intermediates for rubber production according to claim 6, characterized in that: The top of the rotating rod (64) is fixedly connected to a mixing disk (67). The stirring mechanism (6) also includes a connecting frame (68). The connecting frame (68) is fixedly connected to the inner wall of the reaction tank (2). The end of the connecting frame (68) is fixedly connected to a fixing block (69). The lower surface of the fixing block (69) is fixedly connected to a stirring plate (610). The stirring plate (610) is located in the inner cavity of the mixing disk (67). The outer surface of the rotating rod (64) is fixedly connected to a support rod (611). The bottom end of the support rod (611) is fixedly connected to a scraper (612). The lower surface of the scraper (612) is fixedly connected to a scraper blade (613). The scraper blade (613) is rubbed against the upper surface of the fixing disk (61).

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