A reaction kettle

Abstract

The utility model discloses a reation kettle belongs to chemical machinery technical field, including kettle body, control component and semi -continuous feeding assembly, the bottom of kettle body is provided with the discharge gate, the control component includes setting one or more feed port of kettle body, still includes the by -product discharge gate of being connected with kettle body, semi -continuous feeding assembly includes one or more settings semi -continuous feeding port of kettle body, still includes reaction type coil pipe, reaction type coil pipe is located the inside of kettle body, the import of reaction type coil pipe is connected with semi -continuous feeding port, and the export of reaction type coil pipe is close to the bottom of kettle body, the utility model discloses through setting feed port and by -product discharge gate, can add reaction raw material, and discharge by -product, through setting semi -continuous feeding assembly, can add reaction raw material to kettle body, through semi -continuous feeding amount supplement by -product flow -out amount, and then improve the production efficiency of reation kettle.

Description

Technical Field

[0001] This utility model relates to the field of chemical machinery technology, and in particular to a reaction vessel. Background Technology

[0002] Traditional solvent-based polyurethanes release large amounts of volatile organic compounds (VOCs) during production and use, which are difficult to recycle effectively. This not only causes serious environmental pollution and waste of resources, but also poses safety hazards.

[0003] Waterborne polyurethane, using water as the dispersion medium, boasts advantages such as environmental friendliness, safety, excellent mechanical properties, and ease of modification, making it an important development direction for the polyurethane industry. Among them, polyurethane materials synthesized using waterborne polycarbonate polyols as the soft segment exhibit superior comprehensive performance, combining the characteristics of polyether polyols and polyester polyols. They are water-resistant, abrasion-resistant, and have good thermal stability, making them ideal high-end polyurethane raw materials.

[0004] However, the industrial production of waterborne polycarbonate polyols currently still employs a batch process, relying on multiple pieces of equipment (such as reaction vessels, pre-reaction vessels, distillation columns, purification tanks, dehydration vessels, etc.) to operate in stages, which has the following drawbacks:

[0005] 1) Low production efficiency: incomplete reaction, incomplete separation, and low yield;

[0006] 2) High energy consumption: The production line is long, the operation is complex, and the energy consumption is large;

[0007] 3) Environmental and safety risks: Pollution emissions are difficult to control, posing a threat to the health of operators;

[0008] 4) High cost: large investment in equipment and complex maintenance.

[0009] Therefore, it is urgent to optimize production processes and develop efficient, energy-saving, and continuous production equipment to improve reaction efficiency, reduce energy consumption and costs, and at the same time meet environmental protection and safe production requirements. Utility Model Content

[0010] The purpose of this invention is to provide a reaction vessel to solve the problems existing in the prior art. By setting an inlet and a by-product outlet, it is possible to add reaction raw materials and discharge by-products. By setting a semi-continuous feeding component, it is possible to add reaction raw materials to the vessel body and supplement the by-product outflow through the semi-continuous feeding amount, thereby improving the production efficiency of the reaction vessel.

[0011] To achieve the above objectives, this utility model provides the following solution:

[0012] This utility model provides a reaction vessel, including a vessel body, a control component, and a semi-continuous feeding component. The bottom of the vessel body is provided with a discharge port. The control component includes one or more feed ports provided in the vessel body, and also includes a by-product discharge port connected to the vessel body. The semi-continuous feeding component includes one or more semi-continuous feeding ports provided in the vessel body, and also includes a reaction coil located inside the vessel body. The inlet of the reaction coil is connected to the semi-continuous feeding port, and the outlet of the reaction coil is close to the bottom of the vessel body.

[0013] In one embodiment, the semi-continuous feeding assembly further includes a distributor, which includes spray pipes arranged in a crisscross pattern. The distributor is located near the bottom of the vessel body, and the middle part of the distributor is connected to the reaction coil through a liquid inlet pipe. The spray pipes have multiple spray holes.

[0014] In one embodiment, a plurality of feed inlets are provided, including a main feed inlet, a catalyst feed inlet, an auxiliary feed inlet, and a nitrogen inlet distributed at the top of the vessel body, and the by-product outlet includes a distillation and condensation device interface.

[0015] In one embodiment, the control component further includes a vacuum system interface disposed on the vessel body, the vacuum system interface being used to connect to a vacuum system.

[0016] In one embodiment, a plurality of semi-continuous feeding ports are provided, including a semi-continuous feeding nitrogen inlet and a semi-continuous feeding reaction liquid inlet. The semi-continuous feeding nitrogen inlet is connected to the reaction coil through a nitrogen inlet check valve, and the semi-continuous feeding reaction liquid inlet is connected to the reaction coil through a reaction liquid inlet check valve.

[0017] In one embodiment, a heating assembly is further included, which includes a heat-conducting medium inlet, a heat-conducting medium outlet, and a heat-conducting medium pipe. The heat-conducting medium pipe is spirally disposed on the inner wall of the vessel body. The heat-conducting medium inlet passes through the vessel body from the outside and is connected to the bottom of the heat-conducting medium pipe. The heat-conducting medium outlet passes through the vessel body from the outside and is connected to the top of the heat-conducting medium pipe.

[0018] In one embodiment, a cooling component is further included, comprising a cooling medium inlet, a cooling medium outlet, and a cooling medium pipe. The cooling medium pipe is spirally disposed on the inner wall of the vessel body. The cooling medium inlet passes through the vessel body from the outside and is connected to the top of the cooling medium pipe. The cooling medium outlet passes through the vessel body from the outside and is connected to the bottom of the cooling medium pipe.

[0019] In one embodiment, the cooling medium pipe, the reaction coil, and the heat transfer medium pipe are arranged sequentially from the inside to the outside in the radial direction of the vessel body, and the spiral heights of the reaction coil, the heat transfer medium pipe, and the cooling medium pipe are arranged sequentially from high to low.

[0020] In one embodiment, a stirring assembly is also included. The stirring assembly includes a frame, a motor, a reducer, a stirring shaft, and a stirrer. The motor is mounted on the top of the vessel body via the frame. The stirring shaft passes through the vessel body and is provided with a mechanical seal at the penetration position. The top end of the stirring shaft is connected to the motor via the reducer. The portion of the stirring shaft that extends into the vessel body is connected to the stirrer.

[0021] In one embodiment, it further includes an observation window and a maintenance manhole, the observation window being disposed on the top of the vessel body and the maintenance manhole being disposed on the top of the vessel body.

[0022] The present invention achieves the following technical advantages over the prior art:

[0023] This invention, by setting up a feed inlet and a by-product outlet, allows for the addition of reactants through the feed inlet and the discharge of by-products through the by-product outlet. The semi-continuous feeding assembly allows for the replenishment of reactants into the reactor. Simultaneously, the use of a reaction coil ensures that the replenished reactants are heated to approximately the same temperature as the initially added reactants before participating in subsequent reactions. This avoids the reaction being affected by temperature differences between the later-added and earlier-added reactants. Therefore, by supplementing the by-product outflow through semi-continuous feeding, the total amount of reaction in a single reaction within the reactor can be increased, thereby improving the reactor's production efficiency. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 This is a schematic diagram of the overall structure in an embodiment of the present utility model;

[0026] Figure 2 for Figure 1 Detailed structural annotation diagram;

[0027] Figure 3 This is a schematic diagram of the distributor in an embodiment of the present invention;

[0028] The components include: 1. vessel body; 2. heating assembly; 3. cooling assembly; 4. stirring assembly; 5. semi-continuous feeding assembly; and 6. control assembly.

[0029] 11. Cylindrical vessel body structure; 12. Observation window; 13. Inspection manhole;

[0030] 21. Heat transfer medium outlet; 22. Heat transfer medium pipe; 23. Heat transfer medium inlet;

[0031] 31. Cooling medium inlet; 32. Cooling medium pipe; 33. Cooling medium outlet;

[0032] 41. Motor; 42. Reducer; 43. Frame; 44. Mechanical seal; 45. Agitator shaft; 46. Agitator;

[0033] 51. Semi-continuous feeding nitrogen inlet; 52. Nitrogen inlet check valve; 53. Semi-continuous feeding reaction liquid inlet; 54. Reaction liquid inlet check valve; 55. Reaction coil; 56. Liquid inlet pipe; 57. Liquid inlet check valve; 58. Spray pipe; 59. Spray hole;

[0034] 61. First feed inlet; 62. Catalyst feed inlet; 63. Vacuum system interface; 64. Distillation and condensation unit interface; 65. Auxiliary material inlet; 66. Second feed inlet; 67. Nitrogen inlet; 68. Sampling port; 69. Discharge port. Detailed Implementation

[0035] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0036] The purpose of this invention is to provide a reaction vessel to solve the problems existing in the prior art. By setting an inlet and a by-product outlet, it is possible to add reaction raw materials and discharge by-products. By setting a semi-continuous feeding component, it is possible to add reaction raw materials to the vessel body and supplement the by-product outflow through the semi-continuous feeding amount, thereby improving the production efficiency of the reaction vessel.

[0037] To make the above-mentioned objectives, features and advantages of this utility model more apparent and understandable, the utility model will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0038] like Figures 1-3As shown, this utility model provides a reaction vessel, including a vessel body 1, a control component 6, and a semi-continuous feeding component 5. The vessel body 1 can be made of 316L stainless steel and has an integral sealed structure, generally adopting a cylindrical vessel body structure 11. The vessel body 1 itself is resistant to acid and alkali corrosion, high temperature resistance, easy to clean, and has good sealing performance, which can reduce the introduction of impurities, improve product quality, and ensure the service life of the vessel body 1. A discharge port 69 is provided at the bottom of the vessel body 1 for discharging the final product for packaging. The control component 6 includes one or more inlets provided in the vessel body 1, and also includes a by-product outlet connected to the vessel body 1. Reaction raw materials can be added into the vessel body 1 through the inlets, and by-products can be discharged from the vessel body 1 through the by-product outlet. The semi-continuous feeding component 5 includes one or more semi-continuous feeding ports provided in the vessel body 1, through which reaction raw materials can be continuously added into the vessel body 1 to compensate for the reduction in the total amount after the by-products are discharged. The semi-continuous feeding assembly 5 also includes a reaction coil 55, which is located inside the vessel body 1 and is in direct contact with the liquid material (reaction raw materials and reaction intermediates, etc.) inside the vessel body 1. The inlet of the reaction coil 55 is connected to the semi-continuous feeding port, and the outlet of the reaction coil 55 is close to the bottom of the vessel body 1. Thus, when reaction raw materials are added through the semi-continuous feeding port, the reaction raw materials are not directly mixed with the original reaction raw materials, but are mixed after heat exchange through the reaction coil 55.

[0039] This invention, by setting up an inlet and a by-product outlet, allows for the addition of reactants through the inlet and the discharge of by-products through the outlet. The semi-continuous feeding assembly 5 allows for the replenishment of reactants into the reactor body 1. Simultaneously, the reactive coil 55 facilitates heat exchange between the replenished reactants and the original reactants, ensuring that the temperature of the replenished reactants is close to or equal to that of the original reactants before participating in subsequent reactions. This avoids the reaction being affected by temperature differences between the later-added and earlier-added reactants. Therefore, by supplementing the by-product outflow through semi-continuous feeding, the total reaction volume in a single reaction within the reactor body 1 can be increased, thereby improving the production efficiency of the reactor body 1.

[0040] In one embodiment, the semi - continuous feeding assembly 5 further includes a distributor. The distributor includes liquid - spraying pipes 58 arranged in a criss - cross pattern of horizontal and vertical directions. The liquid - spraying pipes 58 can be made of stainless steel. The distributor is close to the bottom of the kettle body 1 so as to reserve a stirring space above the distributor. The liquid - spraying pipes 58 can be arranged in shapes such as a king - shaped or a feng - shaped pattern, so that the liquid - spraying pipes 58 can be distributed within the radial cross - section range of the kettle body 1, improving the mixing convenience of the subsequently added reaction raw materials and the original reaction raw materials. The middle part of the distributor is connected to the reactive coiled pipe 55 through a liquid inlet pipe 56. A liquid inlet check valve 57 is arranged at the connection position between the liquid inlet pipe 56 and the distributor, enabling the semi - continuously added reaction liquid to enter the distributor unidirectionally and preventing the reaction liquid in the kettle body 1 from flowing back. The liquid inlet pipe 56 is an intermediate pipe section connecting the reactive coiled pipe 55 and the distributor, so as to introduce the feed of the reactive coiled pipe 55 into the distributor. The liquid - spraying pipes 58 are provided with a plurality of liquid - spraying holes 59, and the liquid - spraying holes 59 can be evenly distributed on the liquid - spraying pipes 58, so as to disperse and spray the supplemented reaction raw materials through the liquid - spraying holes 59. Regarding the orientation of the liquid - spraying holes 59, they can face downward, sideways or upward. When facing downward, combined with the action of the stirring assembly 4, an upward - flowing trend in the axial direction can be formed, ensuring the full mixing of the supplemented liquid and the original liquid.

[0041] In the production example of aqueous polycarbonate polyol, the pre - reaction liquid is evenly dispersed into the kettle body 1 through the distributor, promoting the full occurrence of transesterification and condensation reactions. Keep the semi - continuous feeding amount consistent with the amount of by - products flowing out and entering the rectification system, thereby improving the production efficiency of the kettle body 1. Through the setting of the distributor, in the reaction stage, the raw materials can be fully distributed to promote the reaction. In the later vacuum and purification stages, nitrogen can be evenly distributed, playing a good role in protection and stripping, improving the product quality and production efficiency.

[0042] In one embodiment, there are multiple feeding ports. The multiple feeding ports include a main - material feeding port, a catalyst feeding port 62, an auxiliary - material adding port 65, and a nitrogen inlet 67 distributed on the top of the kettle body 1. Among them, the main - material feeding port can include a first feeding port 61 and a second feeding port 66 according to the different components of the reaction raw materials. The first feeding port 61 and the second feeding port 66 are respectively used to add different components. The by - product discharge port includes a rectification and condensation device interface 64, which is connected to a rectification and condensation device to condense and recover the discharged by - product gas.

[0043] In the example of waterborne polycarbonate polyol production, the first inlet 61 is used to add dimethyl carbonate or other organic carbonates, the catalyst inlet 62 is used to add catalysts such as organomagnesium or organotin, the auxiliary material inlet 65 is used to add inorganic acid auxiliary materials such as phosphoric acid, and the second inlet 66 is used to add mixed small molecule polyols such as 1,4-butanediol. The nitrogen inlet 67 is used to introduce nitrogen into the reactor body 1 to replace the air inside the reactor body 1 and to provide nitrogen protection, preventing air from entering the reactor body 1, maintaining a slight positive pressure, and avoiding interference with the reaction, thus providing an isolation and protection function.

[0044] In one embodiment, the control component 6 further includes a vacuum system interface 63 disposed on the vessel body 1. The vacuum system interface 63 is used to connect to a vacuum system. When no by-products flow out, the vessel body 1 can be evacuated by turning on the vacuum system to continue the condensation reaction.

[0045] In one embodiment, the semi-continuous feed port includes a semi-continuous nitrogen inlet 51 and a semi-continuous reaction liquid inlet 53. The semi-continuous nitrogen inlet 51 is used to add nitrogen, which serves two purposes: firstly, provides an inert gas environment; and secondly, displaces the reactants in the reaction coil 55. The semi-continuous reaction liquid inlet 53 is used to replenish the reactants. The semi-continuous nitrogen inlet 51 is connected to the reaction coil 55 via a nitrogen inlet check valve 52, ensuring that nitrogen can only enter in one direction and cannot exit. The semi-continuous reaction liquid inlet 53 is connected to the reaction coil 55 via a reaction liquid inlet check valve 54, ensuring that the reactants can only enter in one direction and cannot exit.

[0046] In one embodiment, a heating assembly 2 is also included. The heating assembly 2 includes a heat transfer medium inlet 23, a heat transfer medium outlet 21, and a heat transfer medium pipe 22. The heat transfer medium used can be heat transfer oil, heat transfer water, or other media. The heat transfer medium pipe 22 is spirally arranged on the inner wall of the vessel body 1 and is supported and fixed by the inner wall of the vessel body 1. The heat transfer medium inlet 23 passes through the vessel body 1 from the outside and is connected to the bottom of the heat transfer medium pipe 22. The heat transfer medium outlet 21 passes through the vessel body 1 from the outside and is connected to the top of the heat transfer medium pipe 22. It should be noted that the above connection method of the heat transfer medium pipe 22 is only an example. It should be understood that the heat transfer medium pipe 22 is not limited to the above arrangement. It can also pass through the vessel body 1 and be connected to the heat transfer medium inlet 23 and the heat transfer medium outlet 21, etc. The arrangement of the heat transfer medium inlet 23 at the bottom and the heat transfer medium outlet 21 at the top can adapt to the temperature gradient of the reaction liquid in the height direction within the vessel 1, ensuring uniform and effective heating of the reaction liquid.

[0047] In the example of waterborne polycarbonate polyol production, the heating component 2 is used to control the temperature of the reactor 1 from 50°C to 230°C, and to promote the transesterification polycondensation reaction of dimethyl carbonate, small molecule polyols, etc. in the reactor 1 under the catalysis of organotin or organomagnesium catalysts.

[0048] In one embodiment, a cooling component 3 is also included. The cooling component 3 includes a cooling medium inlet 31, a cooling medium outlet 33, and a cooling medium pipe 32. The cooling medium used can be cooling water or other refrigerants. The cooling medium pipe 32 is spirally arranged on the inner wall of the vessel body 1 and is supported and fixed by the inner wall of the vessel body 1. The cooling medium inlet 31 passes through the vessel body 1 from the outside and connects to the top of the cooling medium pipe 32. The cooling medium outlet 33 passes through the vessel body 1 from the outside and connects to the bottom of the cooling medium pipe 32. It should be noted that the above connection method of the cooling medium pipe 32 is only an example. It should be understood that the cooling medium pipe 32 is not limited to the above arrangement. It can also pass through the vessel body 1 and connect to the cooling medium inlet 31 and the cooling medium outlet 33 respectively. The arrangement of the cooling medium inlet 31 at the top and the cooling medium outlet 33 at the bottom can adapt to the temperature gradient in the height direction of the reaction liquid in the vessel body 1, ensuring uniform and effective cooling of the reaction liquid.

[0049] In the example of waterborne polycarbonate polyol production, the cooling component 3 is used to reduce the temperature of the polycarbonate polyol product to 50°C to 150°C after the reaction is completed, so as to facilitate packaging and sales.

[0050] In one embodiment, the cooling medium pipe 32, the reaction coil 55, and the heat transfer medium pipe 22 are arranged sequentially from the inside to the outside in the radial direction of the vessel body 1. That is, the cooling medium pipe 32 and the heat transfer medium pipe 22 are respectively located on the inner and outer sides of the reaction coil 55. Thus, the reaction coil 55 can be directly preheated and precooled as needed. The spiral heights of the reaction coil 55, the heat transfer medium pipe 22, and the cooling medium pipe 32 are arranged sequentially from high to low. The heat transfer medium pipe 22 can be located within the entire range of the reaction liquid inside the vessel body 1, or the contact range between the heat transfer medium pipe 22 and the reaction liquid can be maximized. This can extend the flow path of the replenished reaction raw materials and ensure that the temperature of the raw materials entering the vessel body 1 through the spray hole 59 of the spray pipe 58 is consistent with the temperature of the original liquid. The height of the heat transfer medium pipe 22 is relatively higher than that of the cooling medium pipe 32. This means that during heating, the heating range can be increased, allowing the reactants to enter the reaction stage as quickly as possible. During cooling, the cooling range can be reduced, allowing the reaction liquid to gradually cool down and obtain the desired product.

[0051] In one embodiment, a stirring assembly 4 is also included. The stirring assembly 4 includes a frame 43, a motor 41, a reducer 42, a stirring shaft 45, and a stirrer 46. The motor 41 is mounted on the top of the vessel body 1 via the frame 43. The stirring shaft 45 penetrates the vessel body 1 and is provided with a mechanical seal 44 at the penetration location to ensure the sealing of the penetration location of the stirring shaft 45. The top end of the stirring shaft 45 is connected to the motor 41 via the reducer 42. The part of the stirring shaft 45 that penetrates into the vessel body 1 is connected to the stirrer 46. Driven by the motor 41 and reduced by the reducer 42, the stirring shaft 45 is rotated, which in turn drives the stirrer 46 to rotate, thereby achieving the stirring and mixing of the reaction liquid in the vessel body 1. The stirrer 46 can be of the form of a paddle, propeller, or turbine, etc., and can perform only circumferential stirring or form axial flow to improve the mixing and stirring effect as needed.

[0052] In the example of waterborne polycarbonate polyol production, the stirring assembly 4 is used to promote the mixing and heat transfer of the reaction solution, improving the efficiency and quality of the transesterification condensation reaction. The stirrer 46 can be a paddle type, divided into three groups, distributed at the upper, middle, and lower parts of the stirring shaft 45, with three blades in each group. This arrangement of the stirrer 46 ensures more uniform and thorough mixing and stirring of the materials within the vessel 1, accelerating the reaction rate and improving the neutralization and purification effects. The mechanical seal 44 improves the sealing effect of the vessel 1, achieving a higher vacuum degree during the vacuum reaction. This allows for water removal at a lower temperature during the dehydration step, thereby reducing the dehydration temperature, shortening the dehydration time, improving dehydration efficiency, and preventing the waterborne polycarbonate polyol from darkening in color.

[0053] In one embodiment, the system also includes an observation window 12 and a maintenance manhole 13. The observation window 12 is located on the top of the vessel body 1, and two or more may be provided depending on the size of the vessel body 1. The maintenance manhole 13 is located on the top of the vessel body 1, facilitating access to the interior of the vessel body 1 for maintenance and inspection without affecting the normal operation of the reaction. Both the observation window 12 and the vessel body 1 are kept sealed during production to avoid the risk of leakage.

[0054] When the reactor of this invention is applied to the preparation of waterborne polycarbonate polyols, it can replace multiple different pieces of equipment, effectively solving problems such as low yield, large plant size, long production line, high energy consumption, high cost and low efficiency, poor environment, and hazards to the safety and health of production personnel during the synthesis of waterborne polycarbonate polyols. The reactor of this invention is scientifically and rationally designed, easy to manufacture, fully functional, low in energy consumption, and compact in structure. The waterborne polycarbonate polyols produced are of stable quality, achieving semi-continuous industrial production, significantly improving the on-site working environment, greatly increasing production efficiency, and significantly increasing the economic benefits for enterprises.

[0055] The present invention provides a water-based polycarbonate polyol production process utilizing the above-mentioned reaction vessel as follows:

[0056] Nitrogen gas is introduced into the vessel body 1 through nitrogen inlet 67 to replace the air inside the vessel body 1 and provide an inert atmosphere;

[0057] 0.1 to 12 tons of dimethyl carbonate raw material are added into the reactor body 1 through the first feed port 61, and 0.1 to 12 tons of small molecule alcohol raw materials such as 1,4-butanediol are added into the reactor body 1 through the second feed port 66. 0.01 kg to 3.00 kg of transesterification polycondensation catalysts such as organomagnesium, organotin, and organoamine are added through the catalyst feed port 62.

[0058] Turn on the stirring assembly 4 and use the heating assembly 2 to heat the reaction liquid in the vessel 1 to 80℃~120℃ to carry out the transesterification reaction. The generated byproduct methanol enters the distillation and condensation device for recycling through the distillation and condensation device interface 64.

[0059] As the mass of the by-product flowing out of the reactor 1 decreases, the semi-continuous feeding component 5 is used to continue adding pre-reaction liquids such as dimethyl carbonate, catalyst, and small molecule polyols into the reactor 1. The liquid is evenly distributed into the reactor 1 through the spray pipe 58 of the distributor to fully react and improve efficiency. The mass of the semi-continuous feeding is controlled to be consistent with the amount of methanol flowing out of the by-product, and the liquid level in the reactor 1 is kept stable at 80% to 90%. The temperature of the reactor 1 is gradually increased to 130°C to 160°C through the heating component 2.

[0060] When the amount of methanol by-product decreases, stop the semi-continuous feeding, close the nitrogen inlet 67 and open the semi-continuous feeding nitrogen inlet 51 at the same time, use nitrogen to replace the pre-reaction liquid in the reaction coil 55, and gradually raise the temperature to 170℃~230℃ to continue the ester exchange condensation reaction.

[0061] Once no byproducts flow out, open the vacuum system interface 63 to evacuate and continue the condensation reaction. Continue the reaction under vacuum conditions for 5 to 25 hours.

[0062] A sample is taken from sampling port 68 for hydroxyl value testing. After the analysis and test are qualified, 0.01 kg to 3.00 kg of phosphoric acid is added from excipient addition port 65. After stirring for 0.5 h to 2.0 h, the product in the reactor body 1 is cooled to 50℃ to 150℃ through cooling component 3, and then packaged through discharge port 69.

[0063] This utility model uses specific examples to illustrate its principles and implementation methods. The above description of the embodiments is only for the purpose of helping to understand the method and core idea of ​​this utility model. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the idea of ​​this utility model. In summary, the content of this specification should not be construed as a limitation of this utility model.

Claims

1. A reaction vessel, characterized in that, include: The vessel body has a discharge port at its bottom. The control component includes one or more feed inlets disposed on the vessel body, and a by-product discharge outlet connected to the vessel body; And a semi-continuous feeding assembly, the semi-continuous feeding assembly including one or more semi-continuous feeding ports disposed in the vessel body, and a reaction coil, the reaction coil being located inside the vessel body, the inlet of the reaction coil being connected to the semi-continuous feeding port, and the outlet of the reaction coil being close to the bottom of the vessel body; The semi-continuous feeding assembly also includes a distributor, which includes spray pipes arranged in a crisscross pattern. The distributor is located near the bottom of the vessel body, and the middle part of the distributor is connected to the reaction coil through a liquid inlet pipe. The spray pipes have multiple spray holes.

2. The reaction vessel according to claim 1, characterized in that: The vessel is equipped with multiple feed inlets, including a main feed inlet, a catalyst feed inlet, an auxiliary feed inlet, and a nitrogen inlet distributed at the top of the vessel. The by-product outlet includes an interface for a distillation and condensation device.

3. The reaction vessel according to claim 1, characterized in that: The control component also includes a vacuum system interface disposed on the vessel body, the vacuum system interface being used to connect to a vacuum system.

4. The reaction vessel according to claim 1, characterized in that: The facility is equipped with multiple semi-continuous feeding ports, each including a semi-continuous nitrogen inlet and a semi-continuous reaction liquid inlet. The semi-continuous nitrogen inlet is connected to the reaction coil via a nitrogen inlet check valve, and the semi-continuous reaction liquid inlet is connected to the reaction coil via a reaction liquid inlet check valve.

5. The reaction vessel according to claim 1, characterized in that: It also includes a heating assembly, which includes a heat-conducting medium inlet, a heat-conducting medium outlet, and a heat-conducting medium pipe. The heat-conducting medium pipe is spirally disposed on the inner wall of the vessel body. The heat-conducting medium inlet passes through the vessel body from the outside and is connected to the bottom of the heat-conducting medium pipe. The heat-conducting medium outlet passes through the vessel body from the outside and is connected to the top of the heat-conducting medium pipe.

6. The reaction vessel according to claim 5, characterized in that: It also includes a cooling component, which includes a cooling medium inlet, a cooling medium outlet, and a cooling medium pipe. The cooling medium pipe is spirally arranged on the inner wall of the vessel body. The cooling medium inlet passes through the vessel body from the outside and is connected to the top of the cooling medium pipe. The cooling medium outlet passes through the vessel body from the outside and is connected to the bottom of the cooling medium pipe.

7. The reaction vessel according to claim 6, characterized in that: The cooling medium pipe, the reaction coil, and the heat transfer medium pipe are arranged sequentially from the inside to the outside in the radial direction of the vessel body, and the spiral heights of the reaction coil, the heat transfer medium pipe, and the cooling medium pipe are arranged sequentially from high to low.

8. The reaction vessel according to claim 1, characterized in that: It also includes a stirring assembly, which includes a frame, a motor, a reducer, a stirring shaft, and a stirrer. The motor is mounted on the top of the vessel body via the frame. The stirring shaft passes through the vessel body and is provided with a mechanical seal at the penetration position. The top end of the stirring shaft is connected to the motor via the reducer. The part of the stirring shaft that extends into the vessel body is connected to the stirrer.

9. The reaction vessel according to claim 1, characterized in that: It also includes an observation window and a maintenance manhole, the observation window being located on the top of the vessel body and the maintenance manhole being located on the top of the vessel body.

Images