Preparation process of ceramic zinc borate flame retardant

Abstract

The invention provides a preparation process of a ceramic zinc borate flame retardant, and relates to the technical field of preparation of zinc borate flame retardants. The preparation process of the ceramic zinc borate flame retardant comprises the following steps: step 1, mixing boric acid and water according to a mass ratio of 1: (1.6-1.9), heating a preparation device to 70 DEG C, adding fatty alcohol-polyoxyethylene ether, and stirring until the fatty alcohol-polyoxyethylene ether is completely dissolved; 2, mixing zinc oxide and boric acid according to the mass ratio of 1: (4-5), stirring for 6-7 hours at the constant temperature of 70-85 DEG C, and then filtering and drying to obtain a zinc borate flame retardant; and 3, mixing the zinc borate flame retardant and the sodium sulfonate modified silane according to a mass ratio of 4: (0.6-1.2), and mechanically grinding to obtain the ceramic zinc borate flame retardant. The zinc borate flame retardant is uniformly mixed during preparation, does not settle and is thorough in reaction.

Description

Technical Field

[0001] The invention relates to the technical field of zinc borate flame retardant preparation, in particular to a preparation process of a ceramic zinc borate flame retardant. Background Art

[0002] Zinc borate flame retardant is a highly effective flame retardant widely used in plastics, rubber, coatings and other fields. Ceramic zinc borate flame retardant can enhance the flame retardant properties of rubber used for wires.

[0003] When preparing ceramic zinc borate flame retardant, zinc oxide is deposited to the bottom of the reactor due to gravity during the reaction process. It can only fully react with boric acid after stirring. The deposition, stirring and reaction are continuously carried out until the reaction is fully completed. Low stirring efficiency will also cause zinc oxide deposition and agglomeration, which is a problem that needs to be solved urgently. Summary of the Invention

[0004] In view of the shortcomings of the existing technology, the present invention provides a preparation process of a ceramic zinc borate flame retardant, which solves the problems of insufficient reaction and zinc oxide precipitation during the preparation of zinc borate.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: A preparation process of a ceramic zinc borate flame retardant comprises the following steps: Step 1: Mix boric acid and water in a mass ratio of 1:1.6-1.9, heat the mixture to 70 degrees Celsius in a preparation device, and add fatty alcohol polyoxyethylene ether while stirring until completely dissolved; Step 2: zinc oxide and boric acid are mixed in a mass ratio of 1:4-5, stirred at a constant temperature of 70-85 degrees Celsius for 6-7 hours, and then filtered and dried to obtain a zinc borate flame retardant; Step 3: mixing the zinc borate flame retardant and the sodium sulfonate modified silane in a mass ratio of 4:0.6-1.2, and then mechanically grinding to obtain a ceramic zinc borate flame retardant; The preparation equipment includes a reactor, which has a hollow main rod rotatably connected to the middle part of the reactor, and multiple groups of hollow stirring rods are installed on the outside of the main rod from top to bottom. A round rod is installed on the outside of each group of stirring rods, and the diameter of the round rod gradually increases from top to bottom. Each of the round rods is rotatably connected to a rotating shaft, and the rotating shaft is provided with evenly distributed reflux blades. A soft shaft is rotatably connected to the inside of each round rod, and both ends of the soft shaft are fixedly connected to the corresponding rotating shaft.

[0006] Preferably, each group of the stirring rods is rotatably connected to a connecting rod, one end of the connecting rod is rotatably passed through the main rod and fixedly connected to bevel gear one, each group of bevel gear one is annularly meshed on the outside of bevel gear two, the other end of the connecting rod is rotatably passed through the round rod and fixedly connected to bevel gear three, the bevel gear three is meshed and connected to bevel gear four, and the bevel gear four is fixedly connected to the soft shaft inside the corresponding round rod.

[0007] Preferably, a driving rod is rotatably connected in the main rod, and the second bevel gear is arranged on the driving rod from top to bottom, and the second bevel gear is rotatably connected in the main rod.

[0008] Preferably, a shell is provided on the top of the reactor, and a gear 1 is rotatably connected to the middle part of the shell. A motor is installed on the top wall of the shell, and the driving end of the motor passes through the shell and is connected to the top surface of the gear 1. The bottom surface of the gear 1 and the driving rod are fixed to each other, and one side of the gear 1 is meshed with the gear 2, and the gear 2 is rotatably connected to the top wall of the shell.

[0009] Preferably, the inner bottom of the shell is rotatably connected to a driving plate, the driving plate and the top end of the main rod are fixed, an inner gear ring is installed on the outer side of the upper surface of the driving plate, and the inner gear ring and gear 1 are meshed with each other.

[0010] Preferably, the bottom end of the main rod is fixedly connected to a scraper rod that fits against the bottom wall of the reactor. The bottom end of the reactor is provided with a discharge port, and a valve is provided on the discharge port.

[0011] Preferably, a first feed port for introducing boric acid and water is provided on one side of the top of the reactor, and a second feed port for introducing zinc oxide is provided on the other side of the top of the reactor.

[0012] Preferably, the reactor has double side walls and a heating plate for temperature control is provided inside the side walls.

[0013] Working principle: During actual use, boric acid and water are mixed in a mass ratio of 1:1.6-1.9, and introduced into the reactor through the feed port 1. The reactor is then heated to 70 degrees Celsius and fatty alcohol polyoxyethylene ether is added and stirred until it is completely dissolved. After dissolution, zinc oxide is introduced into the reactor through the feed port 2. At this time, under a constant temperature of 70-85 degrees Celsius, the motor drives the main rod, round rod, rotating shaft and reflux blade to continue working and stirring for 6-7 hours. When the mixed liquid inside the reactor is stirred, the motor drives gear 2 through gear 1 to rotate the inner gear ring in the shell. When the inner gear ring rotates, the inner gear ring drives the main rod to rotate through the drive plate, and the main rod stirs the solution inside the reactor through the stirring rod and the round rod. At the same time, gear 1 drives bevel gear 2 to rotate through the drive rod When the main rod rotates, bevel gear one drives bevel gear three through the connecting rod, which drives bevel gear four to make the soft shaft rotate in the round rod. When the soft shaft rotates, the rotating shaft rotates on the round rod, and the rotating shaft drives the reflux blades to drive the mixed liquid inside the reactor to mix and stir from bottom to top. When the main rod rotates, the scraper at the bottom of the main rod prevents the zinc oxide that has not reacted completely from being deposited at the bottom of the reactor. At the same time, when the reflux blades rotate, since the spacing between the reflux blades decreases from top to bottom, there is no resistance when the reflux blades stir the liquid at the bottom of the reactor upward, so the zinc oxide that slowly settles at the bottom of the reactor is continuously pushed upward, so that the zinc oxide will not sink and cause a slow reaction, and no sedimentation crystals will appear at the bottom of the reactor. At the same time, it is guaranteed that the evenly mixed reaction solution can realize the effective reaction and make the reaction very sufficient.

[0014] The present invention provides a preparation process for a ceramic zinc borate flame retardant, which has the following beneficial effects: The present invention drives bevel gear two to rotate through gear one through a driving rod, and bevel gear one drives bevel gear three through a connecting rod to drive bevel gear four, so that the soft shaft rotates in the round rod. When the soft shaft rotates, the rotating shaft rotates from the outside to the inside on the round rod, and the rotating shaft drives the reflux blades to drive the mixed liquid inside the reactor to mix and stir from bottom to top along the inner wall of the reactor. When the main rod rotates, the scraper at the bottom of the main rod prevents the deposition of unreacted zinc oxide at the bottom of the reactor. Since the spacing between the reflux blades decreases from top to bottom, when the reflux blades stir the liquid at the bottom of the reactor upward, the liquid flows upward from the inside to the outside, so the zinc oxide slowly settling at the bottom of the reactor is continuously pushed upward, so that the zinc oxide will not sink and cause a slow reaction, and no sedimentation crystallization will appear at the bottom of the reactor, and the reaction is sufficient and uniform. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a main cross-sectional structural diagram of the present invention; Figure 2 It is a top view of the round rod of the present invention; Figure 3 is a cross-sectional view of a return blade of the present invention; Figure 4 for Figure 1 Enlarged view of point A in the middle; Figure 5 for Figure 1 Enlarged view of point B in the middle; Figure 6 for Figure 1 Enlarged view of point C in the middle; Figure 7 Schematic diagram of the mixed liquid flow direction of the present invention.

[0016] Among them, 1. Reactor; 2. Feed port 1; 3. Feed port 2; 4. Motor; 5. Reflux blade; 6. Stirring rod; 7. Main rod; 8. Drive rod; 9. Discharge port; 10. Round rod; 11. Rotating shaft; 12. Flexible shaft; 13. Bevel gear 1; 14. Housing; 15. Internal gear ring; 16. Drive plate; 17. Gear 1; 18. Gear 2; 19. Connecting rod; 20. Bevel gear 2; 21. Bevel gear 3; 22. Bevel gear 4. DETAILED DESCRIPTION

[0017] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0018] Example 1: Refer to Figure 1-6 As shown, an embodiment of the present invention provides a preparation process of a ceramic zinc borate flame retardant, comprising the following steps: Step 1: Mix boric acid and water in a mass ratio of 1:1.6-1.9, heat the mixture to 70 degrees Celsius in a preparation device, and add fatty alcohol polyoxyethylene ether while stirring until completely dissolved; Step 2: zinc oxide and boric acid are mixed in a mass ratio of 1:4-5, stirred at a constant temperature of 70-85 degrees Celsius for 6-7 hours, and then filtered and dried to obtain a zinc borate flame retardant; Step 3: Mixing a zinc borate flame retardant and a sodium sulfonate-modified silane in a mass ratio of 4:0.6-1.2, and then mechanically grinding to obtain a ceramic zinc borate flame retardant. The sodium sulfonate-modified silane can also be combined with a sulfur-containing flame retardant in equal proportions to prepare a ceramic zinc borate flame retardant; Example 2: Refer to Figure 1-6As shown, the embodiment of the present invention provides a preparation process of a ceramic zinc borate flame retardant, including a preparation device, the preparation device including a reactor 1, the inner middle part of the reactor 1 is rotatably connected to a hollow main rod 7, the outer side of the main rod 7 is installed with multiple groups of hollow stirring rods 6 from top to bottom, and each group of stirring rods 6 is installed with a round rod 10 on the outer side, and the diameter of the round rod 10 gradually increases from top to bottom, so that the upstream resistance of the mixed liquid is small when the mixed liquid is stirred, each round rod 10 is rotatably connected to a rotating shaft 11, and the rotating shaft 11 is provided with evenly distributed reflux blades 5, each The round rod 10 is rotatably connected to a flexible shaft 12, and both ends of the flexible shaft 12 are fixedly connected to the corresponding rotating shaft 11. Each group of stirring rods 6 is rotatably connected to a connecting rod 19. One end of the connecting rod 19 rotates through the main rod 7 and is fixedly connected to a bevel gear 13. Each group of bevel gears 13 is annularly meshed with the outer side of the bevel gear 20. The other end of the connecting rod 19 rotates through the round rod 10 and is fixedly connected to a bevel gear 3 21. The bevel gear 3 21 is meshed with a bevel gear 4 22. The bevel gear 4 22 is fixedly connected to the flexible shaft 12 in the corresponding round rod 10. During actual use, boric acid and water are mixed in a mass ratio of 1:1.6-1.9, and introduced into the reactor 1 through the feed port 1-2. After that, the reactor 1 is heated to 70 degrees Celsius and fatty alcohol polyoxyethylene ether is added at the same time, and stirred until it is completely dissolved. After dissolution, zinc oxide is introduced into the reactor 1 through the feed port 2-3. At this time, under a constant temperature of 70-85 degrees Celsius, the motor 4 drives the main rod 7, the round rod 10, the rotating shaft 11 and the reflux blade 5 to continue working and stirring for 6-7 hours. When the mixed liquid inside the reactor 1 is stirred, the motor 4 drives the gear 2 18 through the gear 1 17 to rotate the inner gear ring 15 in the housing 14. When the inner gear ring 15 rotates, the inner gear ring 15 drives the main rod 7 to rotate through the driving plate 16. The main rod 7 stirs the mixed liquid inside the reactor 1 through the stirring rod 6 and the round rod 10. At the same time, the gear 17 drives the bevel gear 2 20 to drive the bevel gear through the driving rod 8. When the gear 11 rotates, the bevel gear 11 drives the bevel gear 3 21 through the connecting rod 19, which drives the bevel gear 4 22 to make the flexible shaft 12 rotate in the round rod 10. When the flexible shaft 12 rotates, the rotating shaft 12 is rotated on the round rod 10, and the rotating shaft 12 drives the reflux blade 5 to drive the mixed liquid inside the reactor 1 to mix and stir from bottom to top. When the main rod 7 rotates, the scraper at the bottom of the main rod 7 prevents the zinc oxide that has not reacted completely from being deposited at the bottom of the reactor 1. At the same time, when the reflux blade 5 rotates, since the spacing between the reflux blades 5 decreases from top to bottom, there is no resistance when the reflux blade 5 stirs the liquid at the bottom of the reactor 1 upward, so the zinc oxide that slowly settles at the bottom of the reactor 1 is continuously pushed upward, so that the zinc oxide will not sink and cause a slow reaction, and no sedimentation crystals will appear at the bottom of the reactor 1, ensuring that the uniformly mixed reaction solution can effectively react and make the reaction very sufficient.

[0019] The main rod 7 is rotatably connected with the driving rod 8. The bevel gear 20 is arranged on the driving rod 8 from top to bottom. The bevel gear 20 is rotatably connected in the main rod 7. The driving rod 8 and the main rod 7 are arranged to be fitted and rotatable. The driving rod 8 rotates in the main rod 7. The driving rod 8 and the main rod 7 are rotatably connected through bearings.

[0020] A shell 14 is provided on the top of the reactor 1, and a gear 17 is rotatably connected to the middle part of the shell 14. A motor 4 is installed on the top wall of the shell 14. The driving end of the motor 4 passes through the shell 14 and is connected to the top surface of the gear 17. The bottom surface of the gear 17 and the driving rod 8 are fixed to each other. One side of the gear 17 is meshed with a gear 2 18, and the gear 2 18 is rotatably connected to the top wall of the shell 14. The motor 4 drives, and combined with the cooperation between the gears, the driving rod 8 rotates when the main rod 7 rotates.

[0021] The inner bottom of the shell 14 is rotatably connected to a drive plate 16, which is fixed to the top of the main rod 7. An inner gear ring 15 is installed on the outer side of the upper surface of the drive plate 16. The inner gear ring 15 and gear 17 are engaged with each other. The inner gear ring 15 can drive the main rod 7 to rotate through the drive plate 16.

[0022] The bottom end of the main rod 7 is fixedly connected to a scraper rod that fits against the bottom wall of the reactor 1 to prevent zinc oxide from depositing and crystallizing at the bottom of the reactor 1, allowing it to react better. A discharge port 9 is provided at the bottom end of the reactor 1. The discharge port 9 is used to discharge the ceramicized zinc borate flame retardant, and a valve is provided on the discharge port 9.

[0023] A feed port 1 2 for introducing boric acid and water is provided on one side of the top of the reactor 1, and a feed port 2 3 for introducing zinc oxide is provided on the other side of the top of the reactor 1.

[0024] The reactor 1 has double side walls and a heating plate for temperature control is provided inside the side walls. The heating plate is used to control the temperature inside the reactor 1 .

[0025] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A preparation process for a ceramic zinc borate flame retardant, characterized in that: The following steps are involved: Step 1: Mix boric acid and water in a mass ratio of 1:1.6-1.9, heat the mixture to 70 degrees Celsius in a preparation device, and add fatty alcohol polyoxyethylene ether while stirring until completely dissolved; Step 2: zinc oxide and boric acid are mixed in a mass ratio of 1:4-5, stirred at a constant temperature of 70-85 degrees Celsius for 6-7 hours, and then filtered and dried to obtain a zinc borate flame retardant; Step 3: mixing the zinc borate flame retardant and the sodium sulfonate modified silane in a mass ratio of 4:0.6-1.2, and then mechanically grinding to obtain a ceramic zinc borate flame retardant; The preparation equipment comprises a reactor (1), wherein a hollow main rod (7) is rotatably connected to the middle of the reactor (1), and multiple groups of hollow stirring rods (6) are installed on the outside of the main rod (7) from top to bottom. A round rod (10) is installed on the outside of each group of stirring rods (6), and the diameter of the round rod (10) gradually increases from top to bottom. Each of the round rods (10) is rotatably connected to a rotating shaft (11), and the rotating shaft (11) is provided with evenly distributed recirculation blades (5). Each of the round rods (10) is rotatably connected to a flexible shaft (12), and both ends of the flexible shaft (12) are fixedly connected to the corresponding rotating shaft (11).

2. The preparation process of a ceramic zinc borate flame retardant according to claim 1, wherein: Each group of the stirring rods (6) is rotatably connected to a connecting rod (19), one end of the connecting rod (19) is rotatably passed through the main rod (7) and fixedly connected to a bevel gear one (13), and each group of the bevel gear one (13) is annularly meshed on the outside of the bevel gear two (20), and the other end of the connecting rod (19) is rotatably passed through the round rod (10) and fixedly connected to a bevel gear three (21), and the bevel gear three (21) is meshed and connected to a bevel gear four (22), and the bevel gear four (22) is fixedly connected to the soft shaft (12) inside the corresponding round rod (10).

3. The preparation process of a ceramic zinc borate flame retardant according to claim 2, characterized in that: The main rod (7) is rotatably connected to a driving rod (8), and the second bevel gear (20) is arranged on the driving rod (8) from top to bottom. The second bevel gear (20) is rotatably connected to the main rod (7).

4. The preparation process of a ceramic zinc borate flame retardant according to claim 3, characterized in that: A shell (14) is provided on the top of the reactor (1), and a gear 1 (17) is rotatably connected to the middle of the shell (14). A motor (4) is installed on the top wall of the shell (14), and the driving end of the motor (4) passes through the shell (14) and is connected to the top surface of the gear 1 (17). The bottom surface of the gear 1 (17) and the driving rod (8) are fixed to each other. One side of the gear 1 (17) is meshed with a gear 2 (18), and the gear 2 (18) is rotatably connected to the top wall of the shell (14).

5. The preparation process of a ceramic zinc borate flame retardant according to claim 4, characterized in that: The inner bottom of the housing (14) is rotatably connected to a driving plate (16), the driving plate (16) and the top end of the main rod (7) are fixed, and an inner gear ring (15) is installed on the outer side of the upper surface of the driving plate (16), and the inner gear ring (15) and gear 1 (17) are meshed with each other.

6. The preparation process of a ceramic zinc borate flame retardant according to claim 1, characterized in that: The bottom end of the main rod (7) is fixedly connected to a scraper rod that fits on the bottom wall of the reactor (1). The bottom end of the reactor (1) is provided with a discharge port (9), and a valve is provided on the discharge port (9).

7. The preparation process of a ceramic zinc borate flame retardant according to claim 1, characterized in that: A first feed port (2) for introducing boric acid and water is provided on one side of the top of the reactor (1), and a second feed port (3) for introducing zinc oxide is provided on the other side of the top of the reactor (1).

8. The preparation process of a ceramic zinc borate flame retardant according to claim 1, characterized in that: The reactor (1) has double-layer side walls, and a heating plate for temperature control is provided inside the side walls.

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