Peroxide diisopropylbenzene condensation reaction production system

Abstract

The utility model relates to the technical field of dicumyl peroxide production, specifically is dicumyl peroxide condensation reaction production system, the dicumyl peroxide condensation reaction production system, including liquid phase catalyst storage tank, refrigerator, liquid phase catalyst storage tank is connected with the reaction kettle through the primary temperature control reverse filter, the reaction kettle is connected with the neutralization kettle through the rectifying column, the neutralization kettle is connected with the backflush filter through the filter press, the backflush filter is connected with the dryer through the crystallizer, the refrigerator is connected with the reaction kettle through the refrigeration liquid storage tank. Through the primary temperature control reverse filter and secondary temperature control reverse filter handle catalyst and solvent respectively, and combine temperature control cover and guarantee that the filtration process temperature is stable, avoid the impurity and gather the blockage because of temperature change.

Description

Technical Field

[0001] This utility model relates to the field of dicumyl peroxide production technology, specifically to a dicumyl peroxide condensation reaction production system. Background Technology

[0002] In the production process of dicumyl peroxide (DCP) condensation reaction, the existing production system in the workshop has two major pain points that seriously affect product quality and production stability.

[0003] Firstly, the filtration and impurity removal effect is poor. Traditional filtration devices lack temperature control, and mechanical and colloidal impurities in the catalyst and solvent easily clog the filter elements. Furthermore, incomplete impurity removal can poison the catalyst, trigger side reactions, and lead to a decrease in product purity. Simultaneously, single filtration devices cannot adapt to the impurity characteristics of different raw materials, resulting in low filtration efficiency and frequent maintenance. Secondly, the precision of reaction cooling control is insufficient. Traditional cooling systems often use a fixed flow rate for liquid supply, failing to adjust in real time according to temperature changes within the reactor. This easily leads to overheating and delayed cooling, increasing the risk of DCP decomposition and resulting in significant energy waste in cooling. In addition, the initial material heating relies on additional energy consumption, failing to effectively utilize waste heat from the production process and increasing production costs. These problems restrict the continuity, safety, and economy of DCP production, necessitating a production system that integrates efficient filtration and impurity removal with precise temperature control. Utility Model Content

[0004] To address the shortcomings of the existing technology, the purpose of this invention is to provide a dicumyl peroxide condensation reaction production system. This system utilizes a primary temperature-controlled reverse filter and a secondary temperature-controlled reverse filter to treat the catalyst and solvent respectively. A temperature control jacket ensures stable temperature during the filtration process, preventing impurities from accumulating and clogging due to temperature changes. The reverse filtration structure, combined with subsequent multi-stage filtration using a filter press and backwash filter, can remove impurities of different particle sizes step by step, ensuring the purity of the raw materials entering the reactor, reducing catalyst poisoning and side reactions, and significantly improving the purity of the DCP product.

[0005] This utility model is achieved using the following technical solution: The dicumyl peroxide condensation reaction production system includes a liquid catalyst storage tank, a refrigerator, a liquid catalyst storage tank connected to a reactor via a primary temperature-controlled reverse filter, a reactor connected to a neutralization vessel via a distillation column, a neutralization vessel connected to a backwash filter via a filter press, a backwash filter connected to a crystallizer and a dryer, and a refrigerator connected to the reactor via a refrigerant storage tank.

[0006] The reactor's coil increases the heat exchange area, and the variable frequency pump precisely regulates the refrigerant flow rate, achieving rapid response and stable control of the reaction temperature. Real-time monitoring ensures that reaction parameters remain within a reasonable range, avoiding the risks of temperature surges and decomposition. The neutralization vessel uniformly mixes the materials and precisely adjusts the pH to neutral to remove residual acid catalysts. The filter press and backwash filter form a multi-stage filtration system, removing impurities of different particle sizes step by step to ensure the purity of subsequent crystallization.

[0007] The dicumyl peroxide condensation reaction production system also includes a solvent storage tank, which is connected to the reactor via a two-stage temperature-controlled reverse filter, and a dryer is connected to the product storage tank via a pipeline.

[0008] The liquid catalyst and solvent storage tanks are designed as sealed tanks, equipped with liquid level monitoring devices, and are used to store catalyst and solvent separately to avoid cross-contamination. This ensures the stability of the raw material storage process, prevents catalyst from getting damp and solvent from evaporating, and provides qualified raw materials for subsequent pretreatment. The primary and secondary temperature-controlled reverse filters have identical structures, both containing filter plates internally, with the raw material inlet located below the filter plate and the outlet above (reverse filtration); an external temperature-controlled sleeve is installed, connected to the distillation column condenser via a temperature-controlled pipe. The reverse filtration method improves impurity interception efficiency and reduces filter element clogging; the temperature-controlled sleeve utilizes waste heat to maintain a stable filtration temperature, preventing impurity accumulation and achieving energy savings, ensuring the effectiveness of raw material pretreatment.

[0009] The primary temperature-controlled reverse filter has a filter plate inside and a temperature-controlled sleeve on the outside.

[0010] The connection between the liquid catalyst storage tank and the primary temperature-controlled reverse filter is located below the filter plate, while the connection between the reactor and the primary temperature-controlled reverse filter is located above the filter plate.

[0011] The distillation column is equipped with a condenser, which is connected to a temperature control sleeve via a temperature control pipe. The condenser is also connected to a two-stage temperature-controlled reverse filter via a temperature control pipe.

[0012] The condenser of the distillation column is connected to the temperature control jacket of the filter via a temperature control pipe, forming a waste heat recovery loop; the column is equipped with distillation packing and temperature monitoring points. It efficiently separates unreacted raw materials and solvents, which can be recycled and reused, reducing raw material consumption; the waste heat from the condenser is used to control the temperature of the filter, achieving energy cascade utilization and reducing energy consumption.

[0013] The reactor is equipped with a reactor coil inside, and a refrigerant storage tank is connected to the reactor coil via a frequency converter pump. A cooling pipe is connected between the frequency converter pump and the reactor coil.

[0014] The refrigerant storage tank is connected to the variable frequency pump via a low-level liquid outlet pipe, and the refrigerant storage tank is connected to the low-level liquid outlet pipe via a high-level liquid outlet pipe.

[0015] The connection between the low-level liquid outlet pipe and the refrigerant storage tank is located at the bottom of the refrigerant storage tank, while the connection between the high-level liquid outlet pipe and the refrigerant storage tank is located at 2 / 3 to 3 / 5 of the vertical wall of the refrigerant storage tank.

[0016] Under normal circumstances, the variable frequency pump feeds liquid through the high-level outlet pipe. When the reactor experiences a sudden abnormal high temperature, liquid is fed through the low-level outlet pipe, increasing the power of the variable frequency pump and rapidly cooling the reactor. The crystallizer efficiently precipitates DCP crystals, improving the crystallization yield; the dryer uses low-temperature vacuum drying to prevent product decomposition; and the product storage tank is sealed with nitrogen to prevent the oxidation and decomposition of DCP during storage, ensuring the quality of the finished product.

[0017] The working principle of this utility model is as follows: In the raw material pretreatment stage, the catalyst in the liquid-phase catalyst storage tank is piped to a primary temperature-controlled reverse filter. The filter plate intercepts mechanical and colloidal impurities, and the temperature control jacket maintains the filtration temperature at 30-40℃ using the waste heat from the distillation column condenser. After filtration, the catalyst is discharged from above the filter plate to the reactor. The solvent in the solvent storage tank is filtered and purified by a secondary temperature-controlled reverse filter, and then sent to the reactor at a controlled temperature of 30-40℃. The filtration accuracy is 5-10μm, and the temperature control fluctuation range is ±2℃.

[0018] The pretreated catalyst, solvent, and α-methylstyrene (AMS) and cumene hydrogen peroxide (CHP) for the condensation reaction stage are fed into the reactor at a molar ratio of CHP:AMS = 1:1.05-1.2. Stirring is started, and refrigerant is pumped into the reactor coils via a variable frequency pump through a refrigerant storage tank. The reaction temperature is controlled at 40-80℃, the pressure at 0.1-0.3MPa, and the pH is maintained at 2-4. The reaction is continued for 2-6 hours. The stirring rate is 50-100 r / min, and the refrigerant flow rate is dynamically adjusted by the variable frequency pump according to the reaction temperature. Emergency cooling is initiated when the temperature exceeds 85℃.

[0019] In the separation and purification stage, the reaction solution is fed into a distillation column, where the top temperature is controlled at 60-80℃. Unreacted AMS and solvent are separated and recycled. The crude product at the bottom of the column enters a neutralization vessel, where alkali is added to adjust the pH to neutral at a temperature of 30-40℃. After neutralization, the material is filtered to remove large salt particles, then passed through a backwash filter (filtration accuracy 0.2-0.5μm) to intercept fine impurities. After filtration, the material is sent to a crystallizer. The crystallizer is cooled to 10-20℃, precipitating DCP crystals. After centrifugation, the crystals are sent to a dryer and dried for 2-4 hours at 50-60℃ and a vacuum of -0.08 to -0.09 MPa.

[0020] After drying, the refined DCP is sent to the product storage tank during the finished product storage stage. It is protected by nitrogen sealing and the storage temperature is ≤25℃.

[0021] Compared with the prior art, the beneficial effects of this utility model are: (1) The catalyst and solvent are treated by a primary temperature-controlled reverse filter and a secondary temperature-controlled reverse filter respectively. Combined with a temperature control sleeve, the temperature of the filtration process is kept stable, and impurities are prevented from accumulating and clogging due to temperature changes. The reverse filtration structure, combined with the multi-stage filtration of the subsequent filter press and backwash filter, can remove impurities of different particle sizes step by step, ensuring the purity of the raw materials entering the reactor, reducing catalyst poisoning and side reactions, and significantly improving the purity of DCP products.

[0022] (2) The refrigeration unit forms a closed-loop temperature control system with the refrigerant storage tank, the variable frequency pump and the reactor coil. It can adjust the refrigerant flow rate in real time according to the reaction temperature, quickly respond to temperature fluctuations, and effectively avoid DCP decomposition caused by temperature surge. At the same time, the waste heat of the distillation column condenser is used to supply energy to the filter temperature control sleeve through the temperature control pipeline, realizing the recovery and utilization of waste heat, reducing energy consumption while ensuring the stability of the initial reaction conditions.

[0023] (3) The structural design of the reverse filter facilitates backwashing maintenance and extends the service life of the filter element; the setting of high and low liquid outlet pipes ensures a stable supply of refrigerant; the application of variable frequency pumps enables energy consumption to be adjusted as needed, thereby improving the continuity and economy of the production system as a whole. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the structure of the dicumyl peroxide condensation reaction production system of this utility model; In the diagram: 1. Liquid catalyst storage tank; 2. Primary temperature-controlled reverse filter; 3. Reactor; 4. Distillation column; 5. Neutralization vessel; 6. Filter press; 7. Backwash filter; 8. Crystallizer; 9. Dryer; 10. Product storage tank; 11. Refrigeration unit; 12. Refrigerant storage tank; 13. Solvent storage tank; 14. Secondary temperature-controlled reverse filter; 15. Filter plate; 16. Reactor coil; 17. Variable frequency pump; 18. High-level liquid outlet pipe; 19. Low-level liquid outlet pipe; 20. Condenser; 21. Temperature control pipe; 22. Cooling pipe; 23. Temperature control jacket. Detailed Implementation

[0025] To make the objectives and technical solutions of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0026] Example 1 like Figure 1As shown, the dicumyl peroxide condensation reaction production system includes a liquid catalyst storage tank 1, a chiller 11, a primary temperature-controlled reverse filter 2 connected to a reactor 3, a distillation column 4 connected to a neutralization vessel 5, a filter press 6 connected to a backwash filter 7, a crystallizer 8 connected to a dryer 9, and a chiller 11 connected to the reactor 3 via a refrigerant storage tank 12. It also includes a solvent storage tank 13, which is connected to the reactor 3 via a secondary temperature-controlled reverse filter 14. The dryer 9 is connected to a product storage tank 10 via a pipeline. The primary temperature-controlled reverse filter 2 has a filter plate 15 inside and a temperature control sleeve 23 on the outside. In the primary temperature-controlled reverse filter 2, the reverse filtration method improves the impurity interception efficiency and reduces filter element clogging. The filtered impurities settle to the bottom of the filter by gravity, reducing impurity deposition on the filter plate 15. The temperature control sleeve 23 utilizes waste heat to maintain a stable filtration temperature, preventing impurity accumulation and achieving energy saving while ensuring the pretreatment effect of the raw materials. The connection between the liquid catalyst storage tank 1 and the primary temperature-controlled reverse filter 2 is located below the filter plate 15, while the connection between the reactor 3 and the primary temperature-controlled reverse filter 2 is located above the filter plate 15. The distillation column 4 is equipped with a condenser 20, which is connected to the temperature control sleeve 23 via a temperature control pipe 21. The reactor 3 is equipped with a reactor coil 16, and the refrigerant storage tank 12 is connected to the reactor coil 16 via a variable frequency pump 17. A cooling pipe 22 connects the variable frequency pump 17 and the reactor coil 16. A low-level outlet pipe 19 connects the refrigerant storage tank 12 to the variable frequency pump 17. The refrigerant storage tank 12 is connected to the low-level outlet pipe 19 via a high-level outlet pipe 18. The connection point between the low-level outlet pipe 19 and the refrigerant storage tank 12 is located at the bottom of the refrigerant storage tank 12, and the connection point between the high-level outlet pipe 18 and the refrigerant storage tank 12 is located at 2 / 3 to 3 / 5 of the vertical wall of the refrigerant storage tank 12.

[0027] The above-mentioned dicumyl peroxide condensation reaction production system includes the following steps during operation: (1) The catalyst in the liquid catalyst storage tank 1 is fed into the first-stage temperature-controlled reverse filter 2 through a pipeline. The filter plate 15 intercepts mechanical impurities and colloidal impurities. The temperature control jacket 23 maintains the filtration temperature at 30-40℃ through the residual heat of the condenser 20 of the distillation column 4. After filtration, the catalyst is discharged from above the filter plate 15 to the reactor 3. The solvent in the solvent storage tank 13 is filtered and purified by the second-stage temperature-controlled reverse filter 14. After the temperature is controlled at 30-40℃, it is sent into the reactor 3. (2) The pretreated catalyst, solvent, α-methylstyrene AMS, and cumene hydrogen peroxide CHP are fed into the reactor 3 at a molar ratio of CHP:AMS=1:1.05-1.2. Stirring is started, and the refrigerant is introduced into the reactor coil 16 through the refrigerant storage tank 12 via the frequency converter pump 17. The reaction temperature is controlled at 40-80℃, the pressure at 0.1-0.3MPa, and the pH value is maintained at 2-4. The reaction is continued for 2-6 hours. (3) The reaction solution is fed into a distillation column 4, where the top temperature is controlled at 60-80℃. Unreacted AMS and solvent are separated and recycled. The crude product at the bottom of the column enters a neutralization vessel 5, where alkali is added to adjust the pH to neutral. The neutralization temperature is 30-40℃. After neutralization, the material is filtered through a filter press 6 to remove large-particle salt impurities, and then filtered through a backwash filter 7 with a filtration accuracy of 0.2-0.5μm to intercept fine impurities. After filtration, the material is fed into a crystallizer 8. The crystallizer 8 is cooled to 10-20℃ to precipitate DCP crystals. After centrifugation, the crystals are sent to a dryer 9 and dried for 2-4 hours at 50-60℃ and a vacuum of -0.08 to -0.09MPa. The dried and purified DCP is sent to a product storage tank 10, which is protected by nitrogen gas and stored at a temperature ≤25℃.

Claims

1. A condensation reaction production system for dicumyl peroxide, characterized in that, The system includes a liquid catalyst storage tank (1), a refrigerator (11), a liquid catalyst storage tank (1) connected to a reactor (3) via a primary temperature-controlled reverse filter (2), a reactor (3) connected to a neutralization vessel (5) via a distillation column (4), a neutralization vessel (5) connected to a backwash filter (7) via a filter press (6), a backwash filter (7) connected to a dryer (9) via a crystallizer (8), and a refrigerator (11) connected to the reactor (3) via a refrigerant storage tank (12).

2. The dicumyl peroxide condensation reaction production system according to claim 1, characterized in that, It also includes a solvent storage tank (13), which is connected to the reactor (3) through a two-stage temperature-controlled reverse filter (14), and a dryer (9) is connected to the product storage tank (10) through a pipeline.

3. The dicumyl peroxide condensation reaction production system according to claim 1, characterized in that, The primary temperature-controlled reverse filter (2) has a filter plate (15) inside and a temperature control sleeve (23) on the outside.

4. The dicumyl peroxide condensation reaction production system according to claim 3, characterized in that, The connection between the liquid phase catalyst storage tank (1) and the primary temperature-controlled reverse filter (2) is located below the filter plate (15), and the connection between the reactor (3) and the primary temperature-controlled reverse filter (2) is located above the filter plate (15).

5. The dicumyl peroxide condensation reaction production system according to claim 3, characterized in that, The distillation column (4) is equipped with a condenser (20) inside, and the condenser (20) is connected to the temperature control sleeve (23) through a temperature control pipe (21).

6. The dicumyl peroxide condensation reaction production system according to claim 1, characterized in that, The reactor (3) is equipped with a reactor coil (16) inside. The refrigerant storage tank (12) is connected to the reactor coil (16) through a variable frequency pump (17). A cooling pipe (22) is connected between the variable frequency pump (17) and the reactor coil (16).

7. The dicumyl peroxide condensation reaction production system according to claim 6, characterized in that, The refrigerant storage tank (12) is connected to the variable frequency pump (17) by a low-level liquid outlet pipe (19), and the refrigerant storage tank (12) is connected to the low-level liquid outlet pipe (19) through a high-level liquid outlet pipe (18).

8. The dicumyl peroxide condensation reaction production system according to claim 7, characterized in that, The connection between the low-level liquid outlet pipe (19) and the refrigerant storage tank (12) is located at the bottom of the refrigerant storage tank (12), and the connection between the high-level liquid outlet pipe (18) and the refrigerant storage tank (12) is located at 2 / 3-3 / 5 of the vertical wall of the refrigerant storage tank (12).

Images