Initiator for initiating free radical reaction and preparation device

By using a composition of dibenzoyl peroxide, azobisisobutyronitrile and other materials and a stirring device with adjustable height, the problems of uneven mixing of liquid initiators and complexity of the device are solved, an efficient and simplified preparation process is achieved, the yield and purity are improved, and it is suitable for large-scale production.

CN120607647APending Publication Date: 2025-09-09YUNNAN HONGSHEN NEW BUILDING MATERIALS TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510683625.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-26
Publication Date
2025-09-09

AI Technical Summary

Technical Problem

The existing liquid initiator preparation process has poor mixing effect, resulting in reduced yield and purity. In addition, the preparation device has a complex structure and cumbersome operation, making it difficult to meet large-scale production needs.

Method used

A combination of dibenzoyl peroxide, azobisisobutyronitrile, solvents and additives is used, combined with an adjustable height electric stirring paddle and a non-powered stirring paddle, and dual mixing and heating control of the reactor and configuration barrel to ensure uniform mixing and cooling treatment.

Benefits of technology

The method achieves efficient mixing of liquid initiators, avoids agglomeration, improves yield and purity, simplifies operation procedures, reduces maintenance costs, and is suitable for large-scale production.

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Abstract

The invention discloses an initiator for initiating free radical reaction and a preparation device. The initiator comprises 15 g of dibenzoyl peroxide, 8 g of azodiisobutyronitrile, 60 g of a solvent A, 10 g of an auxiliary agent B and 7 g of an initiation accelerator C. Dibenzoyl peroxide and azodiisobutyronitrile are used as main free radical initiation components and can be effectively decomposed to generate free radicals in different temperature ranges to initiate reaction. Meanwhile, the device comprises a reaction kettle, and an electric stirring paddle is arranged in the reaction kettle in a height-adjustable manner; a heating pipe is arranged at the periphery of the reaction kettle; the bottom of the reaction kettle is communicated with a spray head through a liquid pump, the spray head is arranged above a configuration barrel, and the configuration barrel is rotatably arranged on an upper barrel frame. The reaction kettle and the preparation barrel are arranged, main initiators can be uniformly mixed in the reaction kettle firstly, then mixed liquid is introduced into quantitative water for secondary mixing, caking or non-uniform mixing of the main initiators is avoided, and non-uniform mixing during secondary mixing is avoided by arranging the spray head and the unpowered stirring paddle.
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Description

Technical Field

[0001] The present invention relates to the technical field of initiators and preparation thereof, in particular to an initiator for initiating free radical reactions and a preparation device thereof. Background Art

[0002] Free radical reactions are widely used in many fields, including polymer synthesis, organic synthesis, and materials science. Liquid initiators, as key substances that trigger free radical reactions, have a direct impact on the reaction rate, efficiency, and product quality.

[0003] Existing liquid initiator preparation processes present numerous challenges. For one thing, poor mixing during the preparation process prevents the raw materials from fully reacting, reducing the yield and purity of the initiator. Furthermore, the raw materials easily agglomerate during the reaction, leading to significant fluctuations in product quality. Furthermore, some preparation equipment is complex, cumbersome to operate, lacks flexibility, and carries high maintenance costs, making it unsuitable for large-scale production. Summary of the Invention

[0004] The main purpose of the present invention is to provide an initiator for initiating free radical reactions and a preparation device, aiming to solve the technical problems of the prior art such as mixing effect, uneven mixing, structural complexity of the preparation device, and poor flexibility.

[0005] To achieve the above object, the present invention provides an initiator for initiating a free radical reaction, comprising: 15 g of dibenzoyl peroxide, 8 g of azobisisobutyronitrile, 60 g of solvent A, 10 g of auxiliary agent B, and 7 g of initiation accelerator C.

[0006] Furthermore, the solvent A is any one or more of ethylene glycol, glycerol, and propylene glycol; The auxiliary agent B is lignin sulfonate; The initiator accelerator C is zinc acetylacetonate.

[0007] Furthermore, the method comprises the following preparation steps: S1. Add solvent A into the reactor, start the stirring system, and stir at a speed of 500 r / min; S2. Slowly add dibenzoyl peroxide, azobisisobutyronitrile, auxiliary agent B, and initiator accelerator C into the reactor in sequence, while stirring; S3. After the addition is complete, continue stirring for 30 minutes to fully mix the ingredients; S4. Turn on the heating system, control the reaction temperature at 60°C, and react for 2 hours to obtain a liquid initiator product.

[0008] An initiator preparation device comprises: a reactor, wherein a height-adjustable electric stirring paddle is provided in the reactor; A heating tube is provided on the periphery of the reactor; The bottom of the reaction kettle is connected to a spray head through a liquid pump. The spray head is arranged above the configuration barrel. The configuration barrel is rotatably arranged on an upper barrel rack.

[0009] Furthermore, there is at least one nozzle, and the total length of the at least one nozzle is less than the radius of the configuration barrel; At least one of the nozzles is arranged on one side of the axis of the configuration barrel.

[0010] Furthermore, the reaction kettle is detachably mounted on a kettle frame, and the kettle frame is height-adjustable and mounted on a supporting frame; The electric stirring paddle is mounted on the stirring motor, and the stirring motor is fixed to the motor frame by screws. The motor frame is height-adjustable and is mounted on the support rod, and the support rod is arranged on the support frame; The heating tube is installed on a tube rack, and the tube rack is sleeved on a supporting frame in an adjustable height.

[0011] Furthermore, the configuration barrel is rotatably mounted on the upper barrel rack via a rotating barrel bearing; The lower part is rotatably embedded in the lower barrel frame through a bearing, and the lower barrel frame is fixed on the upper barrel frame; A non-powered stirring paddle is rotatably provided in the configuration barrel, and the non-powered stirring paddle is mounted on the support frame through a height-adjustable frame; The length of the unpowered stirring paddle is less than the radius of the configuration barrel; The unpowered stirring paddle is arranged on the opposite side of the nozzle.

[0012] Furthermore, a kettle control valve is provided at the bottom of the reactor, and the kettle control valve is detachably connected to the water inlet end of the liquid pump through a nut connector; The water outlet of the liquid pump is connected to the nozzle through a connecting pipe; The liquid pump is installed on a pump frame, and the pump frame is sleeved on a supporting frame in a height-adjustable manner.

[0013] Furthermore, a hollow shaft is provided at the bottom of the configuration barrel, a driven pulley is mounted on the hollow shaft, the driven pulley is sleeved on the driving pulley through a transmission belt, the driving pulley is mounted on the motor through a coupling, and the motor is fixed to the upper barrel frame through a motor bracket.

[0014] Furthermore, a discharge pipe is connected below the hollow shaft, and a barrel control valve is installed on the discharge pipe.

[0015] The beneficial effects of the present invention are embodied in: In the present invention, dibenzoyl peroxide and azobisisobutyronitrile serve as main free radical initiating components, which can effectively decompose to generate free radicals and initiate reactions within different temperature ranges.

[0016] A reactor and a preparation barrel are set up. The main initiator can be mixed evenly in the reactor first, and then a certain amount of water is added to the mixed liquid for secondary mixing to avoid agglomeration or uneven mixing of the main initiator. At the same time, the main initiator after the reactor is prepared can also be passed into the preparation barrel for cooling. A spray nozzle and a non-powered stirring paddle are set. When the barrel rotates at a constant speed, the spray nozzle sprays the initiator evenly on the quantitative liquid surface and stirs it evenly through the non-powered stirring paddle, thereby avoiding uneven mixing during secondary mixing. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention; Figure 2 for Figure 1 Front view of Figure 3 This is a schematic diagram of the structure of the main initiator preparation assembly of the present invention; Figure 4 This is a schematic structural diagram of the primary initiator secondary mixing assembly of the present invention; Figure 5 for Figure 3 sectional view of Figure 6 It is a schematic diagram of the nut connection structure of the present invention.

[0018] Description of reference numerals: 1. Reactor, 2. Heating tube, 3. Electric stirring paddle, 4. Stirring motor, 5. Motor frame, 6. Support rod, 7. Support frame, 8. Kettle frame, 9. Kettle control valve, 10. Nut connector, 11. Liquid pump, 12. Nozzle, 13. Pump frame, 14. Configuration barrel, 15. Upper barrel rack, 16. Barrel control valve, 17. Driven pulley, 18. Motor, 19. Unpowered stirring paddle, 20. Paddle frame, 21. Lower barrel rack, 22. Pipe rack, 23. Drive belt. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. In the absence of conflict, the embodiments in this application and the features in the embodiments can be combined with each other. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0020] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), such directional indications are only used to explain the relative position relationship, movement status, etc. between the various components under a certain specific posture (as shown in the accompanying drawings). If the specific posture changes, the directional indication will also change accordingly.

[0021] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the present invention, the descriptions of "first", "second", etc. are only for descriptive purposes and cannot be understood as indicating or suggesting their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of such features. In addition, the meaning of "and / or" appearing throughout the text includes three parallel schemes. Taking "A and / or B" as an example, it includes scheme A, or scheme B, or schemes in which A and B are satisfied at the same time. In addition, "multiple" refers to more than two. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist.

[0022] The invention discloses an initiator for initiating a free radical reaction, comprising: 15g of dibenzoyl peroxide, 8g of azobisisobutyronitrile, 60g of a solvent A, 10g of an auxiliary agent B, and 7g of an initiation accelerator C.

[0023] The solvent A is any one or more of ethylene glycol, glycerol, and propylene glycol; The auxiliary agent B is lignin sulfonate; The initiator accelerator C is zinc acetylacetonate.

[0024] The method comprises the following preparation steps: S1. Add solvent A into the reactor, start the stirring system, and stir at a speed of 500 r / min; S2. Slowly add dibenzoyl peroxide, azobisisobutyronitrile, auxiliary agent B, and initiator accelerator C into the reactor in sequence, while stirring; S3. After the addition is complete, continue stirring for 30 minutes to fully mix the ingredients; S4. Turn on the heating system, control the reaction temperature at 60°C, and react for 2 hours to obtain a liquid initiator product.

[0025] Dibenzoyl peroxide and azobisisobutyronitrile, as the main free radical initiating components, can effectively decompose to generate free radicals and initiate reactions within different temperature ranges.

[0026] See also Figures 1 to 6As shown, the present invention also provides an initiator preparation device, comprising: a reactor 1, wherein a height-adjustable electric stirring paddle 3 is provided in the reactor 1; The reactor 1 is provided with a heating tube 2 on its periphery; The bottom of the reactor 1 is connected to a spray head 12 via a liquid pump 11 . The spray head 12 is disposed above a configuration barrel 14 . The configuration barrel 14 is rotatably disposed on an upper barrel rack 15 .

[0027] See also Figure 2 As shown, there is at least one nozzle 12, and the total length of at least one nozzle 12 is less than the radius length of the configuration barrel 14; At least one of the nozzles 12 is disposed on one side of the axis of the configuration barrel 14 .

[0028] See also Figure 3 As shown, the reactor 1 is detachably mounted on a reactor frame 8, and the reactor frame 8 is height-adjustable and mounted on a support frame 7; The electric stirring paddle 3 is mounted on the stirring motor 4, and the stirring motor 4 is fixed to the motor frame 5 by screws. The motor frame 5 is height-adjustable and is mounted on the support rod 6, and the support rod 6 is arranged on the support frame 7; The heating tube 2 is installed on a tube rack 22 , and the tube rack 22 is mounted on a support frame 7 in a height-adjustable manner.

[0029] See also Figures 2 to 5 As shown, the configuration barrel 14 is rotatably mounted on the upper barrel frame 15 via a rotating barrel bearing; The lower barrel frame 21 is rotatably mounted on the lower barrel frame 21 through a bearing, and the lower barrel frame 21 is fixed on the upper barrel frame 15; The configuration barrel 14 is rotatably provided with a non-powered stirring paddle 19, and the non-powered stirring paddle 19 is mounted on the support frame 7 by a height-adjustable frame 20; The length of the unpowered stirring paddle 19 is less than the radius of the configuration barrel 14; The unpowered stirring paddle 19 is arranged on the opposite side of the nozzle 12; The blades of the unpowered stirring paddle 19 are rotatably mounted on the paddle shaft.

[0030] See also Figure 4 and 6 As shown, a kettle control valve 9 is provided at the bottom of the reactor 1, and the kettle control valve 9 is detachably connected to the water inlet end of the liquid pump 11 through a nut connector 10; The water outlet of the liquid pump 11 is connected to the nozzle 12 through a connecting pipe; The liquid pump 11 is installed on a pump frame 13 , and the pump frame 13 is sleeved on the support frame 7 in a height-adjustable manner.

[0031] See also Figure 4 As shown, a hollow shaft is provided at the bottom of the configuration barrel 14, and a driven pulley 17 is installed on the hollow shaft. The driven pulley 17 is mounted on the driving pulley through a transmission belt 23. The driving pulley is installed on the motor 18 through a coupling. The motor 18 is fixed to the upper barrel frame 15 through a motor bracket.

[0032] See also Figure 4 As shown, a discharge pipe is connected below the hollow shaft, and a barrel control valve 16 is installed on the discharge pipe.

[0033] How it works When in use, the main initiator is placed in a reaction kettle, mixed by an electric stirring paddle, and heated by a heating tube for reaction; After preparation, add a certain amount of water into the preparation barrel, open the kettle control valve, liquid pump and motor, and the liquid level rotates with the preparation barrel, and the main initiator can be evenly sprayed on the liquid surface; at the same time, the rotation of the liquid surface can drive the blades of the unpowered stirring paddle to rotate around the paddle axis to stir and mix.

[0034] In this solution, a reactor and a configuration barrel are provided, and the main initiator can be mixed evenly in the reactor first, and then the mixed liquid is introduced into a certain amount of water for secondary mixing to avoid agglomeration or uneven mixing of the main initiator; At the same time, the main initiator after the reactor is configured can also be passed into the configuration barrel for cooling; A spray nozzle and a non-powered stirring paddle are set. When the barrel rotates at a constant speed, the spray nozzle sprays the initiator evenly on the quantitative liquid surface and stirs it evenly through the non-powered stirring paddle, thereby avoiding uneven mixing during secondary mixing.

[0035] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An initiator for initiating a free radical reaction, characterized in that ,include: 15g of dibenzoyl peroxide, 8g of azobisisobutyronitrile, 60g of solvent A, 10g of auxiliary agent B, and 7g of initiator accelerator C.

2. The initiator for initiating a free radical reaction according to claim 1, wherein The solvent A is any one or more of ethylene glycol, glycerol, and propylene glycol; The auxiliary agent B is lignin sulfonate; The initiator accelerator C is zinc acetylacetonate.

3. The initiator for initiating a free radical reaction according to claim 1, wherein The method comprises the following preparation steps: S1. Add solvent A into the reactor, start the stirring system, and stir at a speed of 500 r / min; S2. Slowly add dibenzoyl peroxide, azobisisobutyronitrile, auxiliary agent B, and initiator accelerator C into the reactor in sequence, while stirring; S3. After the addition is complete, continue stirring for 30 minutes to fully mix the ingredients; S4. Turn on the heating system, control the reaction temperature at 60°C, and react for 2 hours to obtain a liquid initiator product.

4. An initiator preparation device, characterized in that ,include: A reactor (1), wherein a height-adjustable electric stirring paddle (3) is provided in the reactor (1); A heating tube (2) is provided on the periphery of the reactor (1); The bottom of the reactor (1) is connected to a nozzle (12) via a liquid pump (11). The nozzle (12) is arranged above a configuration barrel (14). The configuration barrel (14) is rotatably arranged on an upper barrel rack (15).

5. An initiator preparation device according to claim 4, characterized in that, There is at least one nozzle (12), and the total length of the at least one nozzle (12) is less than the radius length of the configuration barrel (14); At least one of the nozzles (12) is arranged on one side of the axis of the configuration barrel (14).

6. An initiator preparation device according to claim 5, characterized in that: The reaction kettle (1) is detachably mounted on a kettle frame (8), and the kettle frame (8) is height-adjustable and mounted on a support frame (7); The electric stirring paddle (3) is mounted on the stirring motor (4), the stirring motor (4) is fixed to the motor frame (5) by screws, the motor frame (5) is height-adjustable and is mounted on the support rod (6), and the support rod (6) is arranged on the support frame (7); The heating tube (2) is mounted on a tube rack (22), and the tube rack (22) is mounted on a support frame (7) in a height-adjustable manner.

7. An initiator preparation device according to claim 5, characterized in that: The configuration barrel (14) is rotatably mounted on the upper barrel frame (15) via a rotating barrel bearing; The lower portion is rotatably embedded in the lower barrel frame (21) through a bearing, and the lower barrel frame (21) is fixed on the upper barrel frame (15); A non-powered stirring paddle (19) is rotatably provided in the configuration barrel (14), and the non-powered stirring paddle (19) is mounted on the support frame (7) by means of a height-adjustable frame (20); The length of the unpowered stirring paddle (19) is less than the radius of the configuration barrel (14); The unpowered stirring paddle (19) is arranged on the opposite side of the nozzle (12).

8. An initiator preparation device according to claim 4, characterized in that, A kettle control valve (9) is provided at the bottom of the reactor (1), and the kettle control valve (9) is detachably connected to the water inlet end of the liquid pump (11) via a nut connector (10); The water outlet of the liquid pump (11) is connected to the nozzle (12) via a connecting pipe; The liquid pump (11) is mounted on a pump frame (13), and the pump frame (13) is mounted on a support frame (7) in a height-adjustable manner.

9. An initiator preparation device according to claim 7, characterized in that: A hollow shaft is provided at the bottom of the configuration barrel (14), a driven pulley (17) is mounted on the hollow shaft, the driven pulley (17) is sleeved on the driving pulley via a transmission belt (23), the driving pulley is mounted on the motor (18) via a coupling, and the motor (18) is fixed to the upper barrel frame (15) via a motor bracket.

10. An initiator preparation device according to claim 9, characterized in that: A discharge pipe is connected below the hollow shaft, and a barrel control valve (16) is installed on the discharge pipe.