A reaction kettle for producing phosphorus-modified phenolic resin
By setting up a dehumidification box and air hood driven by a flip motor in the reactor for production of phosphorus-modified phenolic resin, the continuous removal of moisture is achieved, the problem of excessive moisture in the resin polymerization process is solved, and the polymerization quality and production efficiency of the resin are improved.
Patent Information
- Application Number
- CN202411723666.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2044-11-28
AI Technical Summary
Phosphorus-modified phenolic resin produces too much moisture during the polymerization process, affecting the mechanical properties and thermal stability of the resin, resulting in poor polymerization quality.
A reactor for the production of phosphorus-modified phenolic resin was designed. The reactor was turned over with a flip motor, and the two groups of dehumidification boxes were alternately dehumidified, and the molecular sieve was regenerated through the gas hood to achieve continuous removal of moisture.
Effectively remove moisture generated by the reaction, improve the polymerization quality of the resin, meet the needs of continuous production, and ensure reaction uniformity and thermal energy utilization through the design of the stirring and heating sleeve.
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Figure CN119186477B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of phosphorus-modified phenolic resin production, in particular to a reaction kettle for producing phosphorus-modified phenolic resin. Background Art
[0002] Phosphorus-modified phenolic resin is a resin made by introducing phosphorus into the structure of phenolic resin. This modification is mainly to improve the flame retardancy and heat resistance of the resin, and is widely used in electronics, electrical appliances, construction and other fields.
[0003] Since the synthesis of phenolic resin usually involves a polycondensation reaction between phenol and formaldehyde, in this process, the reaction between phenolic hydroxyl and formaldehyde will generate water as a by-product, and phosphoric acid and other phosphorus-based modifiers are used in the polymerization process of phenolic resin, which will further release water through its reaction with phenol or other reactants, so phosphorus-modified phenolic resin will produce more water during the polymerization process, and excessive water will affect the performance of the final resin, resulting in a decrease in the mechanical properties and thermal stability of the resin, so dehumidification is particularly important. In the document (application number: CN202210887169.8), a reactor for processing alkaline-catalyzed phosphorus-modified rosin phenolic resin is disclosed, including a reactor shell, the upper part of the reactor shell is hinged with a reactor cover, the upper part of the reactor cover is provided with a stirring mechanism inside the reactor shell, the bottom of the reactor shell is connected to a feeding mechanism, the lower part of the reactor cover is provided with a cleaning mechanism, and the upper part of the reactor cover is also provided with an automatic pressure relief mechanism. The reaction kettles of this patent and the prior art both perform stirring alone, and do not have a dehumidification function during the reaction, resulting in poor resin polymerization quality. Summary of the invention
[0004] The purpose of the present invention is to solve the above problems and provide a reaction kettle for producing phosphorus-modified phenolic resin.
[0005] In order to achieve the above-mentioned purpose, the present invention specifically adopts the following technical solutions:
[0006] A reactor for producing phosphorus-modified phenolic resin, comprising a frame, wherein a reactor is rotatably mounted inside the frame, the reactor is driven by a flip motor, an upper exhaust pipe is arranged on the top of the reactor, a lower exhaust pipe is arranged on the bottom of the reactor, a feed pipe is arranged on the outside of the reactor, a dehumidification box is fixedly mounted on the inner top and the inner bottom of the reactor, the top and the bottom of the dehumidification box are both baffles, a molecular sieve is stored inside the dehumidification box, an air hood is threadedly connected to the bottom of the dehumidification box, an air hole is arranged at the bottom of the air hood, and the air hole can be opened and closed automatically;
[0007] A plurality of groups of electric heaters are fixedly installed on the outside of the reactor, and the electric heaters are distributed in a circumference. A heating sleeve is sleeved on the outside of the electric heater, and two groups of air cavities are opened inside the heating sleeve. An air inlet pipe is arranged on the outside of the two groups of air cavities, and the two groups of air cavities are respectively connected with two groups of air hoods through exhaust pipes. Solenoid valves are arranged inside the upper exhaust pipe, the lower exhaust pipe, the air inlet pipe and the exhaust pipe. The inside of the air cavity is sealingly and slidably connected with a piston slip ring. Telescopic cylinders are fixedly installed on the top and the bottom of the heating sleeve, and the telescopic end of the telescopic cylinder is connected with the piston slip ring.
[0008] A stirring motor is fixedly installed on the top of the reactor, and a stirring shaft is fixedly connected to the output end of the stirring motor. The stirring shaft passes through the dehumidification box and the air hood. Two groups of stirring blades and a dispersion rod are arranged on the outside of the stirring shaft, and the dispersion rod is located in the dehumidification box.
[0009] Furthermore, the reactor is composed of a reactor body, an upper reactor cover and a lower reactor cover, the upper exhaust pipe is arranged on the upper reactor cover, the lower exhaust pipe is arranged on the lower reactor cover, and the feed pipe is arranged on the reactor body.
[0010] Furthermore, the upper kettle cover and the lower kettle cover are both connected to the reaction kettle body through flanges.
[0011] Furthermore, an inner wall of the reactor body is provided with an inner positioning convex ring, and the inner diameter of the inner positioning convex ring is smaller than the outer diameter of the gas hood.
[0012] Furthermore, a connector is provided at the connecting end of the exhaust pipe and the gas hood, a first connector is provided on the outside of the reactor body, a second connector is provided on the outside of the gas hood, and the connector can be threadedly connected in the first connector and the second connector.
[0013] Furthermore, a top spring is fixedly connected to the bottom of the dehumidification box, and a sealing plate is fixedly connected to the bottom of the top spring, and the sealing plate can seal the air hole. A counterweight ring is arranged between the dehumidification box and the air hood, and the counterweight ring is connected to the sealing plate through a transmission rope. A fixed pulley is arranged at the bottom of the dehumidification box, and the transmission rope changes the transmission direction through the fixed pulley.
[0014] Furthermore, a slide frame is provided at the bottom of the dehumidification box, and a slide block is provided at the top of the sealing plate.
[0015] Furthermore, a plurality of groups of inner guide posts are arranged between the dehumidification box and the air hood, and the plurality of groups of inner guide posts are distributed in a ring shape on the inner side of the counterweight ring.
[0016] Furthermore, the molecular sieve adopts 4A molecular sieve, which is a sodium aluminum silicate with sodium ions as main cations.
[0017] The beneficial effects of the present invention are as follows:
[0018] 1. The present invention arranges dehumidification boxes at both ends of the reactor, and then uses a flip motor to drive the reactor to flip, so that two groups of dehumidification boxes dehumidify alternately, and then the molecular sieve inside the dehumidification box is regenerated by gas through the setting of a gas hood. The two groups of dehumidification boxes are regenerated alternately, which can continuously and effectively remove the moisture generated by the reaction. The resin polymerization quality is high and can meet the needs of continuous production.
[0019] 2. The present invention coordinates stirring by the stirring shaft with flipping of the reactor. Flipping stirring can reduce the dead zone in the reaction vessel, ensure that materials in all areas can effectively participate in the reaction, avoid partial reactants from failing to react fully, and have a good stirring effect.
[0020] 3. The present invention heats the reaction kettle and the inert gas at the same time through an electric heater, which can fully utilize thermal energy, and the heated inert gas can more effectively regenerate the molecular sieve, and the regeneration effect is good. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 The three-dimensional structure of the present invention is shown in FIG. Figure 1 ;
[0022] Figure 2 The three-dimensional structure of the present invention is shown in FIG. Figure 2 ;
[0023] Figure 3 It is a schematic diagram of the cross-sectional structure of the reaction kettle of the present invention;
[0024] Figure 4 It is an exploded view of the reactor of the present invention;
[0025] Figure 5 It is a schematic diagram of the cross-sectional structure of the reaction kettle body of the present invention;
[0026] Figure 6 It is a schematic diagram of the cross-sectional structure of the dehumidification box of the present invention;
[0027] Figure 7 It is a schematic diagram of the cross-sectional structure of the heating sleeve of the present invention.
[0028] Attached figures: 1. frame; 2. flip motor; 3. reactor body; 31. feed pipe; 32. inner positioning convex ring; 33. connection port one; 4. upper reactor cover; 41. upper exhaust pipe; 5. lower reactor cover; 51. lower exhaust pipe; 6. dehumidification box; 61. top spring; 62. sealing plate; 63. air hood; 64. air hole; 65. connection port two; 66. counterweight ring; 67. transmission rope; 68. inner guide column; 7. stirring motor; 71. stirring shaft; 72. stirring blade; 73. dispersion rod; 8. electric heater; 9. heating sleeve; 91. air cavity; 92. air inlet pipe; 93. exhaust pipe; 94. connector; 95. telescopic cylinder; 96. piston slip ring. DETAILED DESCRIPTION
[0029] To make the purpose, technical solution and advantages of the embodiments of the present invention more clear, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention.
[0030] Embodiment 1, as Figure 1-Figure 7 As shown, a reactor for producing phosphorus-modified phenolic resin comprises a frame 1, a reactor is rotatably mounted inside the frame 1, the reactor is driven by a flip motor 2, an upper exhaust pipe 41 is arranged on the top of the reactor, a lower exhaust pipe 51 is arranged on the bottom of the reactor, a feed pipe 31 is arranged on the outside of the reactor, a dehumidification box 6 is fixedly mounted on the inner top and the inner bottom of the reactor, the top and the bottom of the dehumidification box 6 are both baffles, a molecular sieve is stored inside the dehumidification box 6, an air hood 63 is threadedly connected to the bottom of the dehumidification box 6, an air hole 64 is arranged on the bottom of the air hood 63, and the air hole 64 can be opened and closed automatically;
[0031] A plurality of groups of electric heaters 8 are fixedly installed on the outside of the reactor, and the electric heaters 8 are distributed in a circumference. A heating sleeve 9 is sleeved on the outside of the electric heater 8, and two groups of air cavities 91 are opened inside the heating sleeve 9. An air inlet pipe 92 is arranged on the outside of the two groups of air cavities 91. The two groups of air cavities 91 are respectively connected with the two groups of air hoods 63 through an exhaust pipe 93. Solenoid valves are arranged inside the upper exhaust pipe 41, the lower exhaust pipe 51, the air inlet pipe 92 and the exhaust pipe 93. The inside of the air cavity 91 is sealed and slidably connected with a piston slip ring 96. A telescopic cylinder 95 is fixedly installed on the top and the bottom of the heating sleeve 9, and the telescopic end of the telescopic cylinder 95 is connected with the piston slip ring 96.
[0032] A stirring motor 7 is fixedly installed on the top of the reactor, and a stirring shaft 71 is fixedly connected to the output end of the stirring motor 7. The stirring shaft 71 passes through the dehumidification box 6 and the air hood 63. Two sets of stirring blades 72 and a dispersion rod 73 are arranged on the outside of the stirring shaft 71. The dispersion rod 73 is located in the dehumidification box 6.
[0033] When in use, the upper air hole 64 is opened, the lower air hole 64 is closed, the raw materials are poured into the reactor through the feed pipe 31, and then the feed pipe 31 is closed, the equipment is started, the stirring motor 7 drives the stirring shaft 71 to rotate, the stirring shaft 71 drives the stirring blade 72 to rotate, the stirring blade 72 stirs the raw materials, and the moisture generated by the reaction is absorbed by the upper molecular sieve through the upper air hole 64. After a period of time, the flip motor 2 is controlled to be energized, and the flip motor 2 drives the reactor to rotate. When the reactor rotates to a horizontal position, the upper air hole 64 is closed and the lower air hole 64 is opened, and then the raw materials will not flow out through the air hole 64, and then the reactor is flipped 180 degrees. At this time, the original The molecular sieve below continues to absorb moisture, and at the same time, the telescopic cylinder 95 corresponding to the upper kettle cover 4 is controlled to operate, the solenoid valve in the exhaust pipe 93 is opened, the telescopic cylinder 95 pushes the piston sliding ring 96 to slide, and the piston sliding ring 96 pushes the inert gas in the corresponding air cavity 91 into the gas cover 63 through the exhaust pipe 93, and the solenoid valve in the upper exhaust pipe 41 is opened, the inert gas flushes the molecular sieve, and performs gas regeneration treatment on it, and the inert gas is discharged through the upper exhaust pipe 41, that is, while one group of dehumidification boxes 6 is dehumidifying, the molecular sieve in another dehumidification box 6 is regenerated, and the two groups of dehumidification boxes 6 are alternately dehumidified and regenerated, so that the reaction can be continuously carried out, and the production efficiency is high;
[0034] Since the reactor is turned over at intervals, it can cooperate with stirring to reduce the dead zone in the reaction container, ensure that the materials in all areas can effectively participate in the reaction, avoid that some reactants fail to react fully, and improve the stirring effect. At the same time, since the electric heater 8 is located between the heating sleeve 9 and the reactor, the heat generated by the electric heater 8 can be fully utilized to heat the reactor and the inert gas at the same time. The molecular sieve is flushed by the hot inert gas, which can more effectively regenerate the molecular sieve and has a good regeneration effect.
[0035] Since two groups of stirring blades 72 are arranged on the stirring shaft 71, after the reactor is turned over, there will be a group of stirring blades 72 to stir the raw materials, and through the arrangement of the dispersion rod 73, the molecular sieve can be stirred so that the molecular sieve can absorb water more fully, and at the same time the gas regeneration efficiency can be improved.
[0036] Furthermore, the molecular sieve adopts 4A molecular sieve, which is a sodium aluminum silicate with sodium ions as the main cations. It can be regenerated at 150°C and is suitable for heating with dry air or nitrogen flow. The inert gas of the present invention adopts nitrogen. At the same time, the preferred phosphorus-modified phenolic resin ratio of the present invention is: the molar ratio of phenol and formaldehyde is between 1:1.2 and 1:2, the proportion of formaldehyde aqueous solution (37% formaldehyde solution), phosphoric acid or phosphate ester: between 5% and 15% of the total weight, the amount of acidic catalyst (such as sulfuric acid or aluminum chloride) used is 0.5% to 3% of the total reactant mass, the reaction temperature is 150°C, and the heating temperature of the electric heater 8 is 150°C, which can simultaneously meet the reaction and molecular sieve regeneration temperature requirements.
[0037] Embodiment 2, based on the above embodiment, further includes that the reactor consists of a reactor body 3, an upper reactor cover 4 and a lower reactor cover 5, an upper exhaust pipe 41 is arranged on the upper reactor cover 4, a lower exhaust pipe 51 is arranged on the lower reactor cover 5, and a feed pipe 31 is arranged on the reactor body 3.
[0038] Furthermore, the upper kettle cover 4 and the lower kettle cover 5 are both connected to the reaction kettle body 3 through flanges.
[0039] The arrangement of this embodiment facilitates the overall installation of the reactor and makes maintenance easy.
[0040] Embodiment 3, based on the above embodiment, further includes that the inner wall of the reaction kettle body 3 is provided with an inner positioning convex ring 32, and the inner diameter of the inner positioning convex ring 32 is smaller than the outer diameter of the air hood 63. Through this design, the positioning and installation of the dehumidification box 6 and the air hood 63 can be completed quickly, and the installation efficiency is high.
[0041] Embodiment 4, on the basis of the above embodiment, further includes that a connector 94 is provided at the connecting end of the exhaust pipe 93 and the gas hood 63, a connecting port 1 33 is provided on the outer side of the reactor body 3, and a connecting port 2 65 is provided on the outer side of the gas hood 63, and the connector 94 can be threadedly connected in the connecting port 1 33 and the connecting port 2 65. Through this design, the connection between the exhaust pipe 93 and the gas hood 63 can be quickly completed without affecting the assembly of the dehumidification box 6 and the gas hood 63.
[0042] Embodiment 5, on the basis of the above embodiment, further includes: the bottom of the dehumidification box 6 is fixedly connected with a top spring 61, the bottom of the top spring 61 is fixedly connected with a sealing plate 62, the sealing plate 62 can block the air hole 64, a counterweight ring 66 is arranged between the dehumidification box 6 and the air cover 63, the counterweight ring 66 is connected to the sealing plate 62 through a transmission rope 67, and a fixed pulley is arranged at the bottom of the dehumidification box 6, and the transmission rope 67 changes the transmission direction through the fixed pulley.
[0043] After a period of time, the flip motor 2 is powered on, and the flip motor 2 drives the reactor to rotate. When the reactor flips 100°, the reactor is slightly tilted, the counterweight ring 66 below is close to the dehumidification box 6, the transmission rope 67 is relaxed, and the top spring 61 pushes the sealing plate 62 below to block the air hole 64 below. At the same time, the counterweight ring 66 above is moved away from the dehumidification box 6 under the action of gravity, and the sealing plate 62 is driven away from the air hole 64 by the transmission rope 67. Therefore, there is no need for a control structure to automatically open and close the air hole 64. The control is simple, but it should be noted that the single stirring amount cannot be too much, so that when the reactor flips 100°, the raw materials will not be discharged through the air hole 64.
[0044] Furthermore, a slide frame is provided at the bottom of the dehumidification box 6, and a slider is provided at the top of the sealing plate 62, so that the sliding of the sealing plate 62 is more stable.
[0045] Furthermore, a plurality of groups of inner guide posts 68 are provided between the dehumidification box 6 and the air cover 63. The plurality of groups of inner guide posts 68 are distributed in a ring shape on the inner side of the counterweight ring 66, so that the sliding of the counterweight ring 66 is more stable.
[0046] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A reaction kettle for producing phosphorus-modified phenolic resin, comprising a frame (1), characterized in that: A reaction kettle is rotatably mounted inside the frame (1), and the reaction kettle is driven by a turning motor (2). An upper exhaust pipe (41) is arranged on the top of the reaction kettle, and a lower exhaust pipe (51) is arranged on the bottom of the reaction kettle. A feed pipe (31) is arranged on the outside of the reaction kettle. A dehumidification box (6) is fixedly mounted on the top and bottom of the reaction kettle. The top and bottom of the dehumidification box (6) are both baffles. Molecular sieves are stored inside the dehumidification box (6). An air hood (63) is threadedly connected to the bottom of the dehumidification box (6). An air hole (64) is provided at the bottom of the air hood (63), and the air hole (64) can be opened and closed automatically. A plurality of groups of electric heaters (8) are fixedly installed on the outside of the reaction kettle. The electric heaters (8) are distributed in a circumferential manner. A heating sleeve (9) is sleeved on the outside of the electric heater (8). Two groups of air cavities (91) are provided inside the heating sleeve (9). An air inlet pipe (92) is provided on the outside of the two groups of air cavities (91). The two groups of air cavities (91) are respectively connected to two groups of air hoods (63) through an exhaust pipe (93). Solenoid valves are provided inside the upper exhaust pipe (41), the lower exhaust pipe (51), the air inlet pipe (92) and the exhaust pipe (93). A piston sliding ring (96) is sealingly and slidably connected inside the air cavity (91). A telescopic cylinder (95) is fixedly installed on the top and the bottom of the heating sleeve (9). The telescopic end of the telescopic cylinder (95) is connected to the piston sliding ring (96). A stirring motor (7) is fixedly mounted on the top of the reaction kettle, and a stirring shaft (71) is fixedly connected to the output end of the stirring motor (7), the stirring shaft (71) passes through the dehumidification box (6) and the air hood (63), and two groups of stirring blades (72) and a dispersion rod (73) are arranged on the outside of the stirring shaft (71), and the dispersion rod (73) is located in the dehumidification box (6).
2. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 1, characterized in that: The reactor is composed of a reactor body (3), an upper reactor cover (4) and a lower reactor cover (5); the upper exhaust pipe (41) is arranged on the upper reactor cover (4), the lower exhaust pipe (51) is arranged on the lower reactor cover (5), and the feed pipe (31) is arranged on the reactor body (3).
3. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 2, characterized in that: The upper kettle cover (4) and the lower kettle cover (5) are both connected to the reaction kettle body (3) via flanges.
4. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 3, characterized in that: An inner positioning convex ring (32) is provided on the inner wall of the reaction kettle body (3), and the inner diameter of the inner positioning convex ring (32) is smaller than the outer diameter of the gas hood (63).
5. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 4, characterized in that: A connector (94) is provided at the connection end of the exhaust pipe (93) and the gas hood (63); a first connector (33) is provided on the outside of the reaction kettle body (3); a second connector (65) is provided on the outside of the gas hood (63); and the connector (94) can be threadedly connected to the first connector (33) and the second connector (65).
6. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 1, characterized in that: The bottom of the dehumidification box (6) is fixedly connected to a top spring (61), and the bottom of the top spring (61) is fixedly connected to a sealing plate (62), and the sealing plate (62) can block the air hole (64). A counterweight ring (66) is provided between the dehumidification box (6) and the air cover (63), and the counterweight ring (66) is connected to the sealing plate (62) via a transmission rope (67). A fixed pulley is provided at the bottom of the dehumidification box (6), and the transmission rope (67) changes the transmission direction via the fixed pulley.
7. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 6, characterized in that: A sliding frame is provided at the bottom of the dehumidification box (6), and a sliding block is provided at the top of the sealing plate (62).
8. A reaction kettle for producing phosphorus-modified phenolic resin according to claim 7, characterized in that: A plurality of groups of inner guide pillars (68) are arranged between the dehumidification box (6) and the air hood (63), and the plurality of groups of inner guide pillars (68) are distributed in a ring shape on the inner side of the counterweight ring (66).
Citation Information
Patent Citations
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