A device to reduce the risk of material spillage in the TPO rearrangement reaction of photoinitiator

Abstract

This application provides a device for reducing the risk of material spillage in the TPO rearrangement reaction of photoinitiator. The device includes a first reactor with a first upper gas pipe and a second reactor with a second upper gas pipe. The device also includes a connecting pipeline that connects the bottom of the first upper gas pipe to the bottom of the second upper gas pipe. The device for reducing the risk of material spillage in the TPO rearrangement reaction of photoinitiator provided by the embodiments of this application can at least reduce the safety risks caused by material spillage, reduce worker workload, and ensure product quality and working hours.

Description

Technical Field

[0001] This invention relates to the field of chemical production equipment, specifically to a device for reducing the risk of material spillage during the TPO rearrangement reaction of photoinitiator. Background Technology

[0002] TPO, or 2,4,6-trimethylbenzoyl diphenyloxyphosphine, is a highly efficient free radical type I photoinitiator commonly used in UV-curable materials. It boasts advantages such as high efficiency and low yellowing. TPO is widely used in UV-curable coatings, printing inks, UV-curable adhesives, and fiber optic coatings, making it one of the most widely used photoinitiators in the market.

[0003] In the preparation process of TPO, diphenylphosphine chloride is reacted with alcohols such as ethanol or butanol as raw materials, and then rearranged with 2,4,6-trimethylbenzoyl chloride. In actual production, because the chloroalkanes such as chloroethane / chlorobutane generated in the reaction have a certain solubility in the reaction solution, temperature control is required to promote their escape. The release of chloroalkanes such as chloroethane / chlorobutane promotes the forward reaction. However, TPO has a high melting point. If the temperature is too low, TPO will crystallize, preventing gas release and causing the pressure inside the reactor to rise, leading to material overflow. If the temperature is too high, the TPO material will change color, affecting product quality. The reaction itself is exothermic, and improper control will lead to the risk of material overflow. At the same time, the high melting point of TPO makes material overflow difficult to clean up and delays the process.

[0004] See Figure 1 The existing reactor 10 is a single reactor, and the existing technology uses manual monitoring. On-site operators observe the situation inside the reactor in real time, and manually close the tail gas valve 9 when there is a tendency for material to surge, and then reopen it after the bubbles break and the liquid level drops. This technology has the following drawbacks: 1. High safety risk: Manual intervention is delayed, which may lead to uncontrolled reaction, high-temperature material surge and splashing, threatening the safety of operators; 2. Low level of automation: Over-reliance on manual judgment and operation makes it impossible to achieve fully automated production, increasing production costs and safety hazards; 3. In the existing technology, the gases generated during the reaction process are difficult to effectively discharge, which can easily lead to the accumulation of reactants inside the reactor, forming local high-pressure areas, affecting not only reaction efficiency and product quality, but also potentially causing safety accidents; 4. The existing single-reactor reaction design lacks an effective emergency handling mechanism. Once an abnormality occurs in the reaction, it is difficult to transfer the reactants in time, increasing safety risks.

[0005] Therefore, there is an urgent need to develop a device that can reduce the risk of TPO rearrangement reaction material rushing, achieve safe control of the reaction process, and improve production efficiency and product quality. Utility Model Content

[0006] In view of the above-mentioned problems in the prior art, the embodiments of this application propose a device to reduce the risk of material spillage in the TPO rearrangement reaction of photoinitiator. The device can at least reduce the safety risks caused by material spillage, reduce the workload of workers, and ensure product quality and working hours.

[0007] According to one aspect of this application, an apparatus for reducing the risk of material spillage in the rearrangement reaction of photoinitiator TPO is provided. The apparatus includes a first reactor having a first upper gas pipe and a second reactor having a second upper gas pipe. The apparatus also includes a connecting line that connects the bottom of the first upper gas pipe to the bottom of the second upper gas pipe.

[0008] In some embodiments, the connecting pipeline has a first inclined portion, a horizontal portion, and a second inclined portion. The first inclined portion is inclined upward relative to the first upper air pipe at an angle of less than 90 degrees with the first upper air pipe, and the second inclined portion is inclined upward relative to the second upper air pipe at an angle of less than 90 degrees with the second upper air pipe.

[0009] In some embodiments, the ends of the connecting pipeline are respectively connected to a first nitrogen pipeline and a second nitrogen pipeline, a first valve is provided between the first upper gas pipe and the first nitrogen pipeline, and a second valve is provided between the second upper gas pipe and the second nitrogen pipeline.

[0010] In some embodiments, at least one of the first and second reaction vessels is provided with a defoaming agitator.

[0011] In some embodiments, the defoaming mixer has a stirring shaft and a plurality of upper stirring blades and a plurality of lower stirring blades disposed on the stirring shaft.

[0012] In some embodiments, the defoaming agitator further includes one or more of the following features: 1) a stirring blade connected to the end of the stirring blade; 2) a protrusion disposed on the stirring blade; and 3) a perforated defoaming paddle disposed on the stirring blade.

[0013] In some embodiments, both the first and second reactors are provided with an outer jacket, which is connected to a hot water pipe, a circulating water pipe, a steam pipe, and a return water pipe for the hot water and circulating water.

[0014] In some embodiments, the device for reducing the risk of TPO rearrangement reaction of photoinitiator further includes a temperature sensor for detecting the temperature of the reactants and a DSC control system; the DSC control system is connected to the temperature sensor and valves on the pipelines to control the opening and closing of hot water pipelines, circulating water pipelines, steam pipelines and return water pipelines.

[0015] In some embodiments, the device for reducing the risk of TPO rearrangement reaction rushes also includes a buffer tank, with the upper part of the first reactor and the upper part of the second reactor connected to the upper part of the buffer tank via pipelines.

[0016] The beneficial technical effects of this utility model are as follows:

[0017] Through its interconnected dual-reactor design, the equipment in this application significantly reduces safety risks caused by material spillage, eliminates the need for real-time manual supervision, mitigates human error, and ensures product quality and efficient operation. The inclusion of a defoaming agitator further enhances bubble breaking efficiency, reduces spillage incidence, and improves anti-spillage performance. Combined with a temperature sensor and DSC control system, the entire process can be automated, enabling precise temperature control during the reaction and improving production efficiency and product yield. A buffer tank connected to the upper parts of both reactors via pipeline collects any spilled material in extreme conditions, facilitating cleanup and minimizing disruption to production, further enhancing both efficiency and safety. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the embodiments will be briefly described below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. It is worth noting that the various devices / devices are for illustrative purposes only.

[0019] Figure 1 This is a schematic diagram of the structure of a reaction vessel in the prior art.

[0020] Figure 2 This is a schematic diagram of the structure of a reaction apparatus according to an embodiment of this application.

[0021] Figure 3 This is a schematic diagram of the structure of a reaction apparatus according to another embodiment of this application.

[0022] Figure 4 This is a schematic diagram of the structure of a defoaming agitator according to an embodiment of this application.

[0023] Figure 5 This is a schematic diagram of the structure of a defoaming agitator according to another embodiment of this application.

[0024] Figure 6 This is a schematic diagram of the structure of a defoaming agitator according to another embodiment of this application.

[0025] Figure 7 This is a schematic diagram of the structure of a reaction apparatus according to another embodiment of this application.

[0026] Figure 8 This is a schematic diagram of the structure of a reaction apparatus according to another embodiment of this application.

[0027] The reference numerals in the attached drawings are explained as follows: 9. Tail gas valve; 10. Reactor; 11. First reactor; 12. Second reactor; 13. First upper gas pipe; 15. Second upper gas pipe; 17. Connecting pipeline; 19. First inclined section; 21. Horizontal section; 23. Second inclined section; 25. First nitrogen pipeline; 27. Second nitrogen pipeline; 29. ​​First valve; 31. Second valve; 32. Stirring rod; 33. Defoaming stirrer; 34. Stirring shaft; 35. Upper stirring blade; 37. Lower stirring blade; 39. Stirring plate; 41. Protruding column; 43. Perforated defoaming paddle; 45. Outer jacket of the reactor; 47. Buffer tank; 48. Steam valve; 49. Return water valve; 50. Hot water valve; 51. Circulating water valve. Detailed Implementation

[0028] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application are within the scope of protection of this application.

[0029] The following disclosure provides numerous different embodiments or examples for implementing various features of the provided subject matter. Specific examples of devices will be described below to simplify the present invention. Of course, these are merely examples and are not intended to limit the present invention. Reference numerals and / or letters may be repeated in various examples of the present invention. Such repetition is only for brevity and clarity and does not in itself indicate a relationship between the various embodiments and / or configurations discussed.

[0030] Furthermore, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments. In describing specific figures, other devices not shown in the figures may be provided according to actual needs and are not intended to limit this application.

[0031] Figure 2 This is a schematic diagram of a reaction apparatus for reducing the risk of feed rush in the photoinitiator TPO rearrangement reaction according to an embodiment of this application. Figure 2 The specific placement and shape of the various components are merely illustrative for simplicity and clarity, and are not intended to limit this application. Reference Figure 2As shown, according to some embodiments of this application, an apparatus for reducing the risk of material spillage in the rearrangement reaction of photoinitiator TPO is provided. The apparatus includes a first reactor 11, a second reactor 12, and a connecting pipeline 17. The first reactor 11 has a first upper gas pipe 13, and the second reactor 12 has a second upper gas pipe 15. The connecting pipeline 17 connects the bottom of the first upper gas pipe 13 and the bottom of the second upper gas pipe 15. The bottom of the first upper gas pipe 13 can be located below half its height, and the bottom of the second upper gas pipe 15 can be located below half its height. The first upper gas pipe 13 can be located at the top of the first reactor 11, and the second upper gas pipe 15 can be located at the top of the second reactor 12. The first and second upper gas pipes 13 and 15 are exhaust gas pipes and can be connected to an exhaust gas treatment system or other reactors. Both the first reactor 11 and the second reactor 12 are reactors used for the synthesis reaction of photoinitiator TPO. The reaction equipment provided in the embodiments of this application adopts a connected dual-vessel design, in which the two reaction vessels are not used for reaction at the same time. If an accidental material overflow occurs, the material can be directly transferred from the reaction vessel in the process to the other reaction vessel through the connecting pipeline. This can at least reduce the safety risks caused by material overflow, eliminate the need for real-time manual supervision (reducing the workload of workers), eliminate the risk of human error, and ensure product quality and working hours.

[0032] In some embodiments, the inner diameter of the first upper air pipe 13 and the second upper air pipe 17 can be greater than 60 mm, for example, 250 mm. The increased inner diameter of the upper air pipe makes it easier for exhaust gases (such as chloroethane or chlorobutane and other chloroalkanes) to be discharged, reducing accumulation and avoiding bubbles.

[0033] Figure 3 This is a schematic diagram of a reaction apparatus according to another embodiment of this application. (Reference) Figure 3 As shown, in some embodiments, the connecting line 17 may have a first inclined portion 19, a horizontal portion 21, and a second inclined portion 23. The first inclined portion 19 is inclined upward relative to the first upper air pipe 13, and the angle α between the first inclined portion 19 and the first upper air pipe 13 is less than 90 degrees. The second inclined portion 23 is inclined upward relative to the second upper air pipe 15, and the angle β between the second inclined portion 23 and the second upper air pipe 15 is less than 90 degrees. The design of the connecting line with the inclined portion reduces flow resistance when a surge occurs, making it easier for material to enter the connecting line and be collected in the reactor.

[0034] In some embodiments, the connecting pipeline 17 has a hot water heating tape, which wraps around the connecting pipeline 17 to insulate it and prevent the TPO material from cooling and crystallizing in the connecting pipeline 17.

[0035] In some embodiments, the ends of the connecting pipeline 17 are respectively connected to a first nitrogen pipeline 25 and a second nitrogen pipeline 27. A first valve 29 is provided between the first upper gas pipe 13 and the first nitrogen pipeline 25, and a second valve 31 is provided between the second upper gas pipe 15 and the second nitrogen pipeline 27. The added nitrogen pipelines and valves facilitate the cleaning of the connecting pipeline 17.

[0036] from Figure 3 As can be seen, valves are also installed on the first gas supply pipe 13, the second gas supply pipe 15, the first nitrogen line 25, and the second nitrogen line 27. It should be understood that the valves can be set as needed and can be opened or closed according to the reaction process.

[0037] Figure 4 , Figure 5 , Figure 6 The diagram shown is a structural schematic of a defoaming agitator according to some embodiments of this application. It should be understood that... Figure 4 , Figure 5 , Figure 6 The embodiments shown are merely illustrative of some preferred embodiments for clear explanation and are not intended to be limiting. Other structural designs of agitators that can increase defoaming efficiency may also be present.

[0038] In some embodiments, at least one of the first reactor 11 and the second reactor 12 is provided with a defoaming stirrer 33, which means that the stirrer can be used to defoam the reactor. Figure 1 Replace the stirring rod 32 in the middle with Figure 4 / Figure 5 / Figure 6 The defoaming agitator 33 in the middle. The setting of the defoaming agitator can improve the efficiency of breaking up air bubbles, facilitate the release of exhaust gas, reduce the occurrence rate of material slugging, and improve the anti-slugging effect.

[0039] refer to Figure 4 As shown, in some embodiments, the defoaming agitator 33 has a stirring shaft 34 and a plurality of upper stirring blades 35 and a plurality of lower stirring blades 37 disposed on the stirring shaft 34. Figure 4 The image shows two upper stirring blades 35 and two lower stirring blades 37 at the same height. In other embodiments, more upper and lower stirring blades can be provided, and they can be set at different heights (e.g., Figure 7 The reactor is equipped with two upper stirring blades 35 at the same height and four lower stirring blades 37 at different heights. The rotation of the stirring blades can break up the foam generated during the reaction, reducing the risk of material spillage. The arrangement of the upper and lower stirring blades also allows the reactants to form an up-and-down circulating flow within the reactor, further enhancing the breaking efficiency and the mixing effect of the reactants, thereby improving the reaction efficiency.

[0040] refer to Figure 5 As shown, in some embodiments, the defoaming agitator 33 may further include a stirring blade 39 connected to the end of the stirring blades (upper stirring blade 35, lower stirring blade 37). The stirring blades and the stirring blade 39 may be connected by welding. The stirring blade 39 may be connected to the lower stirring blade 37 to form a U-shape, with the opening of the U-shape facing the stirring shaft 34. Alternatively, the stirring blade 39 may be a U-shaped blade alone (e.g., Figure 6 The stirring plate 39 is a U-shaped plate with an opening at the bottom. The stirring plate increases the contact area between the stirrer and the reaction liquid, making the mixing more thorough, improving the defoaming effect, and reducing the risk of material spillage.

[0041] Although the upper stirring blade 35 and the lower stirring blade 37 shown in the figure are both at an angle of 90 degrees to the stirring shaft 34, in reality, both the upper stirring blade 35 and the lower stirring blade 37 can be tilted upwards or downwards relative to the stirring shaft 34.

[0042] refer to Figure 6 As shown, in some embodiments, the defoaming agitator 33 may also include a protrusion 41 disposed on the agitator blade. Figure 6 The diagram shows multiple protrusions 41 provided on the lower stirring blade 37; multiple protrusions 41 may also be provided on the upper stirring blade 35. (Continue to refer to...) Figure 6 As shown, in some embodiments, the defoaming agitator 33 may further include a perforated defoaming paddle 43 disposed on the agitator 39. The perforated defoaming paddle 43 is a sheet-like structure with holes. The protrusions and the perforated defoaming paddles can further increase the efficiency of breaking bubbles, reduce the rate of material slugging, and improve the anti-slugging effect. The position of the protrusions can be adjusted according to the actual reaction conditions to obtain the best effect.

[0043] Figure 7 This is a schematic diagram of a reaction apparatus according to another embodiment of this application. (Reference) Figure 7 As shown, in some embodiments, both the first reactor 11 and the second reactor 12 may be provided with an outer jacket 45. The outer jacket 45 and the reactor (first reactor 11 / second reactor 12) form an annular space. The outer jacket 45 is connected to hot water pipes, circulating water pipes, steam pipes, and hot water and circulating water return pipes. Figure 7 The hot water pipe, circulating water pipe, steam pipe, and return water pipe are not specifically shown, but a steam valve 48 connected to the steam pipe, a hot water valve 50 connected to the hot water pipe, a circulating water valve 51 connected to the circulating water pipe, and a return water valve 49 connected to the return water pipe are shown. By controlling the opening and closing of each valve, the flow of hot water, circulating water, and steam in the outer jacket 45 of the reactor is controlled, thereby controlling the temperature of the reactor to meet the needs of different reaction stages.

[0044] In some embodiments, the reaction apparatus may further include a temperature sensor (not shown in the figure) for detecting the temperature of the reactants and a DSC control system (not shown in the figure). The DSC control system is connected to the temperature sensor and valves (steam valve 48, hot water valve 50, circulating water valve 51, and return water valve 49) on the pipelines to control the opening and closing of the hot water pipeline, circulating water pipeline, steam pipeline, and return water pipeline. The installation of the temperature sensor and the DSC control system enables the present application to achieve full-process automation, realize precise temperature control of the reaction process, and improve production efficiency and product qualification rate. The DSC control system includes components such as a central processing unit, memory, and input / output interfaces. The DSC control system receives signals from the temperature sensor through the input interface and controls the opening and closing of the valves on the pipelines through the output interface. The DSC control system can automatically adjust the opening and closing of valves on hot water pipes, circulating water pipes, steam pipes, and return water pipes based on the preset reaction temperature curve and the actual temperature feedback from the temperature sensor to control the temperature inside the reactor. When the actual temperature is lower than the preset temperature, the DSC control system will open the valves on the hot water pipes or steam pipes to introduce hot water or steam into the outer jacket of the reactor, thereby increasing the temperature inside the reactor. When the actual temperature is higher than the preset temperature, the DSC control system will open the valves on the circulating water pipes to introduce circulating water into the outer jacket of the reactor, thereby decreasing the temperature inside the reactor.

[0045] Figure 8 This is a schematic diagram of a reaction apparatus according to another embodiment of this application. (Reference) Figure 8 As shown, in some embodiments, the reaction apparatus may further include a buffer tank 47, with the upper part of the first reaction vessel 11 and the upper part of the second reaction vessel 12 connected to the upper part of the buffer tank 47 via pipelines. The buffer tank is used to collect spilled materials in extreme situations, facilitating collection and cleanup, and will not have a significant impact on production, further improving production efficiency and safety.

[0046] The device provided in this application for reducing the risk of material spillage in the TPO rearrangement reaction of photoinitiators can fundamentally reduce the risk of material spillage and achieve full automation without the need for manual monitoring of the reaction. Even if material spillage occurs due to accidents, the existence of a second reaction vessel and / or buffer tank for material collection will not have a significant impact on production, greatly improving production efficiency.

[0047] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. An apparatus for reducing the risk of TPO rearrangement reaction surge in a photoinitiator, characterized in that, include: A first reactor having a first upper air pipe and a second reactor having a second upper air pipe; Connect the pipeline to the bottom of the first upper air pipe and the bottom of the second upper air pipe.

2. The apparatus of claim 1, wherein, The connecting pipeline has a first inclined portion, a horizontal portion, and a second inclined portion. The first inclined portion is inclined upward relative to the first upper air pipe at an angle of less than 90 degrees with the first upper air pipe, and the second inclined portion is inclined upward relative to the second upper air pipe at an angle of less than 90 degrees with the second upper air pipe.

3. The apparatus of claim 1, wherein, The two ends of the connecting pipeline are respectively connected to a first nitrogen pipeline and a second nitrogen pipeline. A first valve is provided between the first upper gas pipe and the first nitrogen pipeline, and a second valve is provided between the second upper gas pipe and the second nitrogen pipeline.

4. The apparatus of claim 1, wherein, At least one of the first and second reaction vessels is equipped with a defoaming agitator.

5. The apparatus of claim 4, wherein, The defoaming agitator has a stirring shaft and multiple upper stirring blades and multiple lower stirring blades disposed on the stirring shaft.

6. The apparatus of claim 5, wherein, The defoaming agitator also includes one or more of the following features: 1) A stirring blade connected to the end of the stirring blade; 2) Protrusions set on the stirring blades; 3) Perforated defoaming paddles set on the stirring plate.

7. The apparatus of claim 1, wherein, Both the first and second reactors are equipped with an outer jacket, which is connected to a hot water pipe, a circulating water pipe, a steam pipe, and a return water pipe for both hot water and circulating water.

8. The apparatus of claim 7, wherein, It also includes a temperature sensor for detecting the temperature of the reactants and a DSC control system; The DSC control system is connected to temperature sensors and valves on the pipelines to control the opening and closing of the hot water pipeline, the circulating water pipeline, the steam pipeline, and the return water pipeline.

9. The device according to claim 1, characterized in that, It also includes a buffer tank, and the upper parts of the first reactor and the second reactor are connected to the upper part of the buffer tank via pipelines.

Images