Preparation method of composite photosensitive polymeric material for photocuring 3D printing
By using inert gas to adjust the temperature and reduce pressure distillation in a single reactor, the problem of contamination of composite photosensitive materials during the transfer reaction in multiple containers is solved, and high-quality photocuring 3D printing and molding is achieved, avoiding secondary treatment .
Patent Information
- Application Number
- CN202411355885.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2025-02-14
AI Technical Summary
In the prior art, composite photosensitive materials are easily contaminated during the transfer reaction in multiple containers, resulting in a decrease in the quality of the microfluidic chip formed by photocuring 3D printing, and requires secondary processing.
By preheating and temperature adjustment in a single reactor through inert gas, the modification of polydimethylsiloxane and silane coupling agent, the stirring and mixing of photoinitiators, photosensitizers, dispersants, and thickening agents are achieved, and the Distillation under reduced pressure to obtain a polydimethylsiloxane photocuring slurry.
It effectively avoids contamination of reaction products due to frequent transfer, improves the photocuring and forming quality of composite photosensitive polymer materials, and avoids the need for secondary treatment.
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Figure CN119425569A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of 3D printing, and in particular to a method for preparing a composite photosensitive polymer material for photocuring 3D printing. Background Art
[0002] A microfluidic chip refers to a chemical or biological laboratory built on a chip of a few square centimeters. The manufacturing technology of microfluidic chips mainly uses ultraviolet lithography, nanoimprinting, injection molding, 3D printing and other technologies. 3D printed microfluidic chips are gradually being used due to their better precision and lower cost.
[0003] 3D printed microfluidic chips usually use photocuring technology, which requires composite photosensitive materials. Conventional composite photosensitive materials usually need to be mixed and reacted successively at different ambient temperatures by basic raw materials and multiple additives at different reaction temperatures during the preparation process. Therefore, it is necessary to replace multiple reaction containers according to the additive addition steps to carry out multiple reactions at different temperatures. Although this method can prepare photocurable composite photosensitive materials, the product needs to be transferred multiple times in this process to adapt to the preparation reaction process under different conditions. During the transfer process, the mixed material is easily contaminated and a small amount of impurities are present in the product. After photocuring molding, some impurities are easily solidified on the surface of the microfluidic chip and reduce the quality of the microfluidic chip, which is easy to affect the displacement experiment.
[0004] Therefore, the conventional method of preparing composite photosensitive materials by multi-container transfer reaction is easily contaminated during the transfer process, resulting in the need for secondary treatment of the flow channel surface after the microfluidic chip is formed by photocuring 3D printing. Summary of the invention
[0005] The purpose of the present invention is to provide a method for preparing a composite photosensitive polymer material for photocuring 3D printing, so as to solve the technical problem in the prior art that the composite photosensitive material is easily contaminated due to the need for transfer reaction preparation in multiple containers, resulting in the need for secondary treatment after the photocuring 3D printing microfluidic chip is formed.
[0006] In order to solve the above technical problems, the present invention specifically provides the following technical solutions:
[0007] A method for preparing a composite photosensitive polymer material for photocuring 3D printing, comprising the following steps:
[0008] Step 100, preheating the reaction kettle with inert gas and placing a certain amount of polydimethylsiloxane into the reaction kettle, heating it to a preset temperature with inert gas and stirring it, and at the same time, spraying a certain amount of silane coupling agent into the reaction kettle to obtain modified polydimethylsiloxane after stirring for a preset time;
[0009] Step 200, after the modified polydimethylsiloxane in the reactor is stirred and cooled to a preset value by using an inert gas, a certain amount of photoinitiator, photosensitizer, dispersant, and thickener are added to the reactor and stirred, and at the same time, stirred at a set temperature rise rate to obtain a mixed solution after stirring for a preset time;
[0010] Step 300, using an inert gas to cool the mixed solution in the reactor to a preset value, and using a vacuum distiller to adjust the pressure in the reactor to a preset negative pressure value, distilling the mixed solution in the reactor, and cooling it to room temperature after the distillation reaches a preset time, so as to discharge and filter to obtain polydimethylsiloxane photocuring slurry.
[0011] As a preferred embodiment of the present invention, in step 100, the gas-heat-stirring treatment method for stirring and modifying polydimethylsiloxane and a silane coupling agent comprises:
[0012] Inert gas is transported into the reactor through pipelines so that the reactor is filled with inert gas to form gas protection, and hot inert gas is introduced into the hollow stirring blades in the reactor so that the temperature of the stirring blades is raised to a set temperature;
[0013] A fixed amount of polydimethylsiloxane and a silane coupling agent are sequentially added to the feeder on the reactor, and the polydimethylsiloxane and the silane coupling agent enter the pipeline from the feeder, and are carried by the airflow transported into the reactor and sprayed into the reactor;
[0014] The polydimethylsiloxane and silane coupling agent sprayed into the reaction kettle are in an environment protected by inert gas, and the polydimethylsiloxane and silane coupling agent are stirred by stirring blades after entering the reaction kettle;
[0015] At the same time, the stirring blade heated by the hot inert gas quickly heats the polydimethylsiloxane and the silane coupling agent to reach the set reaction temperature and continues stirring until the set time ends to obtain modified polydimethylsiloxane.
[0016] As a preferred embodiment of the present invention, in step 200, the gas-heat-preserved stirring treatment method for stirring and mixing the modified polydimethylsiloxane with the photoinitiator, the photosensitizer, the dispersant, and the thickener comprises:
[0017] After the polydimethylsiloxane modification is completed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and stirring is continued for a certain period of time so that the temperature of the modified polydimethylsiloxane reaches the same temperature as that of the stirring blade;
[0018] Continue to add a certain amount of photoinitiator, photosensitizer, dispersant and thickener to the feeder on the reactor in sequence, and the photoinitiator, photosensitizer, dispersant and thickener enter the pipeline from the feeder in sequence, and are carried by the airflow transported into the reactor and sprayed into the reactor;
[0019] The photoinitiator, photosensitizer, dispersant and thickener sprayed into the reaction kettle are in an environment protected by inert gas, and the photoinitiator, photosensitizer, dispersant and thickener are stirred by stirring blades after entering the reaction kettle;
[0020] At the same time, the inert gas introduced into the stirring blade gradually heats up at a set temperature rise rate, and stirs and heats the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant, and thickener until the set stirring time ends to obtain a mixed solution.
[0021] As a preferred embodiment of the present invention, in step 300, the method for implementing the reduced pressure distillation reaction of the mixed solution includes:
[0022] After the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant and thickener are uniformly mixed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and the stirring is continued for a certain period of time so that the temperature of the mixed solution reaches the same temperature as the stirring blade;
[0023] The negative pressure distiller on the reactor is used to evacuate the interior of the reactor to make the pressure inside the reactor reach the set pressure value, and the temperature and pressure state in the reactor are maintained for a set time. At the same time, the stirring blade rotates slowly to stir the mixed solution in the reactor for a set time;
[0024] After the reduced pressure distillation reaches the set time, the temperature of the inert gas introduced into the stirring blade is reduced to the preset temperature and stirring is continued for a certain period of time to reduce the temperature of the mixed solution to room temperature, and the product is discharged from the reactor and filtered to obtain polydimethylsiloxane photocuring slurry.
[0025] As a preferred embodiment of the present invention, in step 100, the polydimethylsiloxane modification stirring reaction temperature is 100-150° C., the stirring speed is 250-680 rpm, and the stirring time is 20-70 min.
[0026] As a preferred embodiment of the present invention, in step 200, the basic reaction temperature of modified polydimethylsiloxane with photoinitiator, photosensitizer, dispersant and thickener is 30-50°C, the stirring heating rate is 2-10°C / min, and the stirring time is 5-30min.
[0027] As a preferred embodiment of the present invention, in step 300, the vacuum degree of the mixed solution in the reactor is 0.01-20 kPa, the reaction time is 1-10 hours, and the product inside the reactor is cooled to room temperature after the reaction.
[0028] As a preferred embodiment of the present invention, a reaction device for stirring and modifying polydimethylsiloxane and a silane coupling agent, stirring and mixing the modified polydimethylsiloxane with a photoinitiator, a photosensitizer, a dispersant, and a thickener, and distilling the mixed solution under reduced pressure comprises:
[0029] A reactor, wherein a protection pipeline is provided on the reactor for conveying inert gas protection into the reactor;
[0030] Two stirring shafts are symmetrically arranged in the reactor and rotate synchronously;
[0031] A temperature regulating pipeline, partly arranged in the two stirring shafts, the temperature regulating pipeline comprises an intake manifold, two stirring pipelines, and a return manifold which are rotatably connected in sequence, the intake manifold and the return manifold are respectively arranged at both ends of the two stirring shafts and fixed outside the reactor, the two stirring pipelines are arranged in the stirring shafts and partially exposed in the reactor, and the part of the stirring pipeline exposed in the reactor extends outward to form a stirring blade arranged around the stirring shaft;
[0032] A feeder, arranged on the reactor and connected to the protection pipeline, used to feed the reaction material into the protection pipeline and spray it into the reactor along with the inert gas flow;
[0033] A negative pressure mechanism, arranged on the reactor and connected to the temperature regulating pipeline, is used to extract gas from the reactor to generate negative pressure and return the extracted inert gas to the temperature regulating pipeline;
[0034] When stirring reaction is required, after the stirring shaft rotates the stirring pipeline to stir, the protection pipeline is opened to introduce inert gas protection and hot gas is introduced into the temperature control pipeline to heat the stirring pipeline. At the same time, a quantitative reaction material is added to the reactor through the feeder and the protection pipeline, and then the protection pipeline is closed, and the negative pressure mechanism adjusts the pressure in the reactor according to the reaction requirements to continuously stir for a preset time to obtain the target product.
[0035] As a preferred solution of the present invention, the stirring pipeline includes a plurality of junction boxes, and a plurality of blade tubes distributed around the axis of each of the adjacent junction boxes are arranged to communicate with each other, and the axially adjacent blade tubes are arranged in an annular pattern, and the blade tubes are fixed on the stirring shaft in a U shape;
[0036] The stirring shaft is provided with a plurality of chambers, the plurality of chambers are used to fix a plurality of junction boxes, a plurality of fixing holes are provided on the side wall of the stirring shaft, each of the fixing holes is connected to the corresponding chamber, and the blade tube extends out of the stirring shaft through the fixing hole and is fixed;
[0037] Both ends of the stirring shaft are provided with rotating holes, and the two rotating holes are respectively connected to the two chambers on the outside. The branch ends of the intake manifold and the return manifold are sealed and rotatably inserted into the rotating holes and are respectively rotatably connected to the two junction boxes on the outside.
[0038] As a preferred embodiment of the present invention, the feeder comprises two feeding hoppers with sealing covers, the bottoms of the two feeding hoppers are connected with feeding manifolds, and the feeding manifolds are connected with the protection pipeline to add solid materials and liquid materials into the protection pipeline respectively;
[0039] The protection pipeline is provided with two boosting pipelines through a one-way valve, and the two boosting pipelines are respectively provided on the two feeding hoppers, so as to introduce inert gas into the feeding hopper for boosting the pressure when adding materials;
[0040] The negative pressure mechanism includes a negative pressure pump arranged on the reactor, and the negative pressure pump is respectively provided with a negative pressure pipe and a recovery pipe, the negative pressure pipe is connected with a vacuum distillation component, and the vacuum rectification component is connected to the top of the reactor, which is used to change the vacuum degree of the reactor and collect the distilled liquid, and the recovery pipe is connected to the return gas manifold to recover or discharge the extracted inert gas.
[0041] Compared with the prior art, the present invention has the following beneficial effects:
[0042] The present invention adopts a single reactor temperature control reaction method, uses inert gas to provide a protective environment for the reaction materials in the reactor, and adjusts the reaction temperature in the reactor by changing the temperature of the inert gas, so that the raw materials of the composite photosensitive polymer material can react under different temperature conditions in the same reactor, thereby effectively avoiding the contamination of the reaction products due to frequent transfer, improving the quality of the composite photosensitive polymer material after light-curing molding, and eliminating the need for secondary treatment. BRIEF DESCRIPTION OF THE DRAWINGS
[0043] In order to more clearly illustrate the implementation methods of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for the implementation methods or the description of the prior art. Obviously, the drawings in the following description are only exemplary, and for ordinary technicians in this field, other implementation drawings can be derived from the provided drawings without creative work.
[0044] Figure 1A flowchart of a method for preparing a composite photosensitive polymer material provided by an embodiment of the present invention;
[0045] Figure 2 A schematic diagram of the structure of a gas-heated stirring treatment device for a method for preparing a composite photosensitive polymer material provided by an embodiment of the present invention;
[0046] Figure 3 A schematic diagram of the structure of the stirring shaft portion of the gas-heated stirring treatment device of the method for preparing the composite photosensitive polymer material provided by an embodiment of the present invention;
[0047] Figure 4 A schematic diagram of the structure of the blade tube portion of the gas-heat-preserved stirring treatment device of the method for preparing the composite photosensitive polymer material provided by an embodiment of the present invention;
[0048] Figure 5 A schematic diagram of the structure of the shunt pipe portion of the gas-heat-preserved stirring treatment device of the method for preparing the composite photosensitive polymer material provided by an embodiment of the present invention;
[0049] Figure 6 A schematic diagram of the structure of the corrugated shell portion of the gas-insulated heat-stirring treatment device of the method for preparing the composite photosensitive polymer material provided by an embodiment of the present invention;
[0050] Figure 7 A schematic structural diagram of the feeder portion of the gas-heated stirring treatment device of the method for preparing the composite photosensitive polymer material provided in an embodiment of the present invention.
[0051] The numbers in the figure represent the following:
[0052] 1-reactor; 2-stirring shaft; 3-temperature control pipeline; 4-feeder;
[0053] 11-protection pipeline; 12-heat exchanger; 13-gas tank; 14-negative pressure pump; 21-chamber; 22-fixing hole; 23-rotating hole; 31-intake manifold; 32-mixing pipeline; 33-return air manifold; 41-feeding hopper; 42-feeding manifold;
[0054] 111-boosting pipeline; 112-control valve; 131-compressor; 132-pressure reducing valve; 133-four-way selection valve; 134-air supply pipeline; 135-waste discharge pipeline; 141-negative pressure pipe; 142-recovery pipe; 143-vacuum distillation assembly; 321-merging box; 322-leaf tube; 323-diverter pipe; 324-core column; 325-corrugated shell; 326-annular mouth; 327-chuck. DETAILED DESCRIPTION
[0055] 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 described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0056] like Figure 1 As shown, the present invention provides a method for preparing a composite photosensitive polymer material for photocuring 3D printing, comprising the following steps:
[0057] Step 100, preheating the reaction kettle with inert gas and placing a certain amount of polydimethylsiloxane into the reaction kettle, heating it to a preset temperature with inert gas and stirring it, and at the same time, spraying a certain amount of silane coupling agent into the reaction kettle to obtain modified polydimethylsiloxane after stirring for a preset time;
[0058] Step 200, after the modified polydimethylsiloxane in the reactor is stirred and cooled to a preset value by using an inert gas, a certain amount of photoinitiator, photosensitizer, dispersant, and thickener are added to the reactor and stirred, and at the same time, stirred at a set temperature rise rate to obtain a mixed solution after stirring for a preset time;
[0059] Step 300, using an inert gas to cool the mixed solution in the reactor to a preset value, and using a vacuum distiller to adjust the pressure in the reactor to a preset negative pressure value, distilling the mixed solution in the reactor, and cooling it to room temperature after the distillation reaches a preset time, so as to discharge and filter to obtain polydimethylsiloxane photocuring slurry.
[0060] In the method, a silane coupling agent is added while the polydimethylsiloxane is stirred, so that the silane coupling agent can be more evenly mixed into the polydimethylsiloxane for reaction, thereby improving the uniformity of the surface modification of the polydimethylsiloxane and the speed of the modification treatment. After the modification is completed, the temperature is lowered and a photoinitiator, a photosensitizer, a dispersant, and a thickener are added to heat and stir to obtain a mixed solution, and then the mixed solution is subjected to reduced pressure distillation to obtain a polydimethylsiloxane photocurable slurry by filtration.
[0061] Compared with the existing method of preparing photosensitive materials by transferring separate reactors, the present method uses the temperature of the inert gas to adjust the reaction temperature in the reaction reactor, thereby achieving the functions of completing the modification of polydimethylsiloxane, the stirring and mixing reaction of the modified polydimethylsiloxane with a photoinitiator, a photosensitizer, a dispersant, and a thickener to produce a mixed solution, and the distillation of the mixed solution to obtain polydimethylsiloxane photocurable slurry in the same reactor, thereby eliminating the need for frequent transfer of products, making the preparation of polydimethylsiloxane photocurable slurry more convenient.
[0062] Specifically, in step 100, the gas-heat stirring treatment method for stirring and modifying polydimethylsiloxane and a silane coupling agent includes:
[0063] Inert gas is transported into the reactor through pipelines so that the reactor is filled with inert gas to form gas protection, and hot inert gas is introduced into the hollow stirring blades in the reactor so that the temperature of the stirring blades is raised to a set temperature;
[0064] A fixed amount of polydimethylsiloxane and a silane coupling agent are sequentially added to the feeder on the reactor, and the polydimethylsiloxane and the silane coupling agent enter the pipeline from the feeder, and are carried by the airflow transported into the reactor and sprayed into the reactor;
[0065] The polydimethylsiloxane and silane coupling agent sprayed into the reaction kettle are in an environment protected by inert gas, and the polydimethylsiloxane and silane coupling agent are stirred by stirring blades after entering the reaction kettle;
[0066] At the same time, the stirring blade heated by the hot inert gas quickly heats the polydimethylsiloxane and the silane coupling agent to reach the set reaction temperature and continues stirring until the set time ends to obtain modified polydimethylsiloxane.
[0067] The polydimethylsiloxane modified stirring reaction temperature is 100-150° C., the stirring speed is 250-680 rpm, and the stirring time is 20-70 min.
[0068] Specifically, in step 200, the gas-heat stirring treatment method for stirring and mixing the modified polydimethylsiloxane with the photoinitiator, the photosensitizer, the dispersant, and the thickener includes:
[0069] After the polydimethylsiloxane modification is completed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and stirring is continued for a certain period of time so that the temperature of the modified polydimethylsiloxane reaches the same temperature as that of the stirring blade;
[0070] Continue to add a certain amount of photoinitiator, photosensitizer, dispersant and thickener to the feeder on the reactor in sequence, and the photoinitiator, photosensitizer, dispersant and thickener enter the pipeline from the feeder in sequence, and are carried by the airflow transported into the reactor and sprayed into the reactor;
[0071] The photoinitiator, photosensitizer, dispersant and thickener sprayed into the reaction kettle are in an environment protected by inert gas, and the photoinitiator, photosensitizer, dispersant and thickener are stirred by stirring blades after entering the reaction kettle;
[0072] At the same time, the inert gas introduced into the stirring blade gradually heats up at a set temperature rise rate, and stirs and heats the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant, and thickener until the set stirring time ends to obtain a mixed solution.
[0073] The basic reaction temperature of the modified polydimethylsiloxane with the photoinitiator, photosensitizer, dispersant and thickener is 30-50°C, the stirring heating rate is 2-10°C / min, and the stirring time is 5-30min.
[0074] Specifically, in step 300, the method for implementing the reduced pressure distillation reaction of the mixed solution includes:
[0075] After the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant and thickener are uniformly mixed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and the stirring is continued for a certain period of time so that the temperature of the mixed solution reaches the same temperature as the stirring blade;
[0076] The negative pressure distiller on the reactor is used to evacuate the interior of the reactor to make the pressure inside the reactor reach the set pressure value, and the temperature and pressure state in the reactor are maintained for a set time. At the same time, the stirring blade rotates slowly to stir the mixed solution in the reactor for a set time;
[0077] After the reduced pressure distillation reaches the set time, the temperature of the inert gas introduced into the stirring blade is reduced to the preset temperature and stirring is continued for a certain period of time to reduce the temperature of the mixed solution to room temperature, and the product is discharged from the reactor and filtered to obtain polydimethylsiloxane photocuring slurry.
[0078] The vacuum degree of the mixed solution in the reactor during reduced pressure distillation is 0.01-20 kPa, the reaction time is 1-10 hours, and the product inside the reactor is cooled to room temperature after the reaction is completed.
[0079] In order to complete the three steps of reaction in one reactor, Figure 2 As shown, a gas-heat-preserved stirring reaction device is provided, which is used to stir and modify polydimethylsiloxane and a silane coupling agent, stir and mix the modified polydimethylsiloxane with a photoinitiator, a photosensitizer, a dispersant, and a thickener, and decompress and distill the mixed solution, specifically comprising:
[0080] Reactor 1, the reactor 1 is provided with a protection pipeline 11 for conveying inert gas protection into the reactor 1;
[0081] Two stirring shafts 2 are symmetrically arranged in the reactor 1 and rotate synchronously;
[0082] The temperature regulating pipeline 3 is partially arranged in the two stirring shafts 2. The temperature regulating pipeline 3 includes an intake manifold 31, two stirring pipelines 32, and a return air manifold 33 which are rotatably connected in sequence. The intake manifold 31 and the return air manifold 33 are respectively arranged at both ends of the two stirring shafts 2 and fixed outside the reactor 1. The two stirring pipelines 32 are arranged in the stirring shafts 2 and partially exposed in the reactor 1. The portion of the stirring pipeline 32 exposed in the reactor 1 extends outward to form a stirring blade arranged around the stirring shaft 2.
[0083] The feeder 4 is arranged on the reactor 1 and connected to the protection pipeline 11, and is used to feed the reaction materials into the protection pipeline 11 and spray them into the reactor 1 along with the inert gas flow;
[0084] A negative pressure mechanism is provided on the reactor 1 and connected to the temperature regulating pipeline 3, and is used to extract gas from the reactor 1 to generate negative pressure and return the extracted inert gas to the temperature regulating pipeline 3;
[0085] When stirring reaction is required, after the stirring shaft 2 rotates the stirring pipeline 32 for stirring, the protection pipeline 11 is opened to introduce inert gas protection and hot gas is introduced into the temperature control pipeline 3 to heat the stirring pipeline 32. At the same time, a quantitative reaction material is added to the reactor 1 through the feeder 4 and the protection pipeline 11, and then the protection pipeline 11 is closed, and the negative pressure mechanism adjusts the pressure in the reactor 1 according to the reaction requirements to continuously stir for a preset time to obtain the target product.
[0086] The gas heat preservation stirring treatment device in this embodiment mainly forms the stirring pipe 32 of the temperature regulating pipe 3 into the stirring blade on the stirring shaft 2, so that when the stirring shaft 2 rotates, the stirring pipe 32 replaces the stirring blade to stir the materials in the reactor 1, and the stirring pipe 32 is introduced with hot gas from the intake manifold 31, so that the stirring pipe 32 stirs and heats the materials in the reactor 1 to provide a reaction temperature environment;
[0087] The feeder 4 is connected to the protection pipeline 11 to realize the inert gas delivery and material delivery, thereby avoiding frequent opening of the cover for delivery and affecting the inert gas protection. The feeder 4 cooperates with the protection pipeline 11 to spray the silane coupling agent on the polydimethylsiloxane for stirring, so as to meet the requirement of adding the silane coupling agent while stirring the polydimethylsiloxane.
[0088] The negative pressure mechanism is connected to the reactor 1 and can extract the gas in the reactor 1 to reduce the pressure inside the reactor 1 according to demand, thereby meeting the demand for achieving reduced pressure distillation in the reactor 1.
[0089] Compared with the existing sealed heating and stirring device, the gas-protected heat stirring treatment device provided by the present method can use inert gas to provide protection and heat or cool it in a circulating flow in the stirring pipeline 32, so that during the stirring process, constant temperature stirring, temperature rise stirring, and rapid cooling functions can be achieved to meet the needs of continuous stirring reaction of polydimethylsiloxane and silane coupling agent at a temperature of 100-150°C, and meet the needs of heating and stirring of modified polydimethylsiloxane and photoinitiator, photosensitizer, dispersant, and thickener at 30-50°C and a heating rate of 2-10°C / min, and meet the needs of maintaining distillation stirring at 50-80°C under a reduced pressure environment.
[0090] Based on the above embodiments, it can be known that the stirring pipeline 32 needs to exchange heat with the material in the reactor 1 to adjust the reaction temperature, and also needs to replace the stirring blade to complete the stirring work. Based on this, the following preferred embodiments are provided.
[0091] like Figure 3 , Figure 4 As shown, the stirring pipeline 32 includes a plurality of junction boxes 321, and a plurality of blade tubes 322 distributed around the axis of the junction boxes 321 are arranged between two adjacent junction boxes 321, and the blade tubes 322 adjacent to each other in the axial direction are arranged in an annular pattern, and the blade tubes 322 are fixed on the stirring shaft 2 in a U shape;
[0092] The stirring shaft 2 is provided with a plurality of chambers 21, and the plurality of chambers 21 are used to fix a plurality of junction boxes 321. A plurality of fixing holes 22 are provided on the side wall of the stirring shaft 2, and each fixing hole 22 is connected to a corresponding chamber 21, and the blade tube 322 extends out of the stirring shaft 2 through the fixing hole 22 and is fixed;
[0093] Both ends of the stirring shaft 2 are provided with rotating holes 23, which are respectively connected to the two outer chambers 21. The branch ends of the intake manifold 31 and the return manifold 33 are sealed and rotatably inserted into the rotating holes 23 and are respectively rotatably connected to the two outer junction boxes 321.
[0094] Specifically, the plurality of vane tubes 322 and the plurality of junction boxes 321 form a parallel passage with multiple junction points, so that the airflow entering the intake manifold 31 can flow through all the vane tubes 322 in sequence to the return manifold 33 to heat the vane tubes 322, so that the vane tubes 322 can heat the material during the stirring process as stirring blades to maintain the reaction temperature of the material or reduce the temperature of the material;
[0095] The stirring shaft 2 adopts a multi-piece assembly structure, that is, the stirring pipeline 32 can be placed between multiple parts of the stirring shaft 2 and locked and fixed. Therefore, in order to facilitate the fixing of the stirring pipeline 32 on the stirring shaft 2, a chamber 21 is set in the stirring shaft 2 to fix the junction box 321, and a fixing hole 22 is set to fix the blade tube 322 and a rotating hole 23 is set to facilitate the intake manifold 31 and the return manifold 33 to enter and connect to the junction box 321.
[0096] Since the area of the material stirred by the single blade tube 322 is effective during the rotation, the stirring effect produced is average. Therefore, in order to improve the stirring effect provided by the blade tube 322 instead of the stirring blade, the following preferred embodiments are provided.
[0097] like Figure 5 As shown, a plurality of shunt pipes 323 are provided between the U-shaped inner walls of the leaf tube 322, and the middle diameter of the shunt pipe 323 is larger than the diameter at both ends thereof;
[0098] The U-shaped ends of the blade tube 322 and the fixed points of the two junction boxes 321 form a fixed rotation angle, so that the blade tube 322 is tilted on the stirring shaft 2.
[0099] Specifically, the shunt pipe 323 is arranged between the U-shaped inner walls of the blade tube 322, thereby effectively improving the stirring effect of the stirring pipeline 32, and due to the addition of the shunt pipe 323, the total contact area between the stirring pipeline 32 and the material is increased, which effectively increases the heat exchange rate, thereby increasing the temperature rise or temperature drop rate, that is, improving the preparation efficiency, and the thickening in the middle can further increase its contact area;
[0100] The U-shaped ends of the blade tube 322 and the fixed points of the two junction boxes 321 form a fixed rotation angle, so that the blade tube 322 is inclined with respect to the rotation direction, thereby improving the strength of the blade tube 322 and effectively preventing the blade tube 322 from bending during the stirring process.
[0101] Based on the above embodiment, further, Figure 6 As shown, the shunt pipe 323 includes a core column 324, and a corrugated shell 325 is coaxially mounted on the outside of the core column 324. The ends of the core column 324 and the corrugated shell 325 form an annular opening 326, and the shunt pipe 323 is connected to the leaf tube 322 through the annular opening 326;
[0102] A plurality of chucks 327 are equidistantly arranged on the core column 324 , and the plurality of chucks 327 are respectively placed in a plurality of wave crests of the corrugated shell 325 , so as to form a wavy flow channel between the core column 324 and the corrugated shell 325 .
[0103] Specifically, the diverter tube 323 adopts a double-layer design, allowing the gas to flow from the gap between the core column 324 and the corrugated shell 325, and the chuck 327 can change the direction of the airflow so that the airflow can flow through each wave crest of the corrugated shell 325 in turn, thereby extending the flow and increasing the contact area between the diverter tube 323 and the material, further improving the adjustment speed of temperature rise and temperature drop.
[0104] Based on the above embodiments, the feeder 4 can deliver the reaction materials into the protection pipeline 11 and add them into the reactor 1 along with the air flow, which can effectively reduce the air content. Based on this, the following preferred embodiments are provided.
[0105] like Figure 2 , Figure 7 As shown, the feeder 4 includes two feeding hoppers 41 with sealing covers, and the bottoms of the two feeding hoppers 41 are connected to a feeding manifold 42, and the feeding manifold 42 is connected to the protection pipeline 11 to add solid materials and liquid materials into the protection pipeline 11 respectively;
[0106] Two pressurizing pipelines 111 are arranged on the protection pipeline 11 through a one-way valve. The two pressurizing pipelines 111 are respectively arranged on two feeding hoppers 41 so as to introduce inert gas into the feeding hopper 41 for pressurization when adding materials.
[0107] Specifically, after adding materials into the feeding hopper 41 and closing the sealing cover, the one-way valve is opened, and the protection pipeline 11 conveys gas to the feeding hopper 41 through the booster pipeline 111 upstream of the airflow. Then, the material in the feeding hopper 41 enters the downstream of the protection pipeline 11 under the action of pressure, and is sprayed into the reactor 1 along with the airflow, so that the material is not concentrated, thereby increasing the stirring reaction speed.
[0108] Gas is introduced into the temperature control pipeline 3 for temperature control, and inert gas is introduced into the protection pipeline 11 for protection. Using the same inert gas for temperature control and protection can effectively reduce gas supply equipment. Based on this, the following preferred embodiments are provided.
[0109] like Figure 2 As shown, the hot gas introduced into the temperature regulating pipeline 3 is an inert gas, and a control valve 112 is provided at the end of the protection pipeline 11. The control valve 112 is connected to the intake manifold 31 to divert part of the inert gas in the intake manifold 31 to be introduced into the reactor 1 for protection;
[0110] The reactor 1 is provided with a heat exchanger 12 , and a portion of the intake manifold 31 is connected to the heat exchanger 12 , so that the inert gas in the intake manifold 31 is heated or cooled by contact heat exchange.
[0111] Specifically, the protection line 11 is controlled to open and close by the control valve 112, and is opened when inflation protection and feeding are required, and the protection line 11 is connected to the intake manifold 31 through the control valve 112, that is, the inert gas in the protection line 11 uses the inert gas in the temperature regulating line 3, even if the inert gas injected into the reactor 1 has the same temperature as the inert gas in the stirring line 32, thereby effectively reducing the effect of feeding on the temperature, and being able to quickly increase the temperature in the reactor 1 during initial use;
[0112] The heating or cooling of the inert gas is achieved by connecting the intake manifold 31 to the heat exchanger 12 . The heat exchanger 12 can provide heating or cooling heat exchange, that is, it can meet the temperature rise and temperature drop requirements of the stirring pipeline 32 .
[0113] The inert gas needs to be temporarily stored at the reactor 1 to facilitate the recycling of the temperature control pipeline 3 and the timely use of the protection pipeline 11. Based on this, the following preferred embodiments are provided.
[0114] like Figure 2 As shown, a gas tank 13 for storing inert gas is arranged outside the reactor 1, and a compressor 131 and a pressure reducing valve 132 are arranged on the gas tank 13, and a four-way selection valve 133 is arranged on the compressor 131. The pressure reducing valve 132 and the four-way selection valve 133 are respectively connected to the main end of the intake manifold 31 and the main end of the return manifold 33 to circulate the inert gas;
[0115] The four-way selector valve 133 is also provided with an air supply pipeline 134 and a waste discharge pipeline 135 . The air supply pipeline 134 is used to supply inert gas, and the waste discharge pipeline 135 is used to discharge waste gas.
[0116] Specifically, the gas tank 13 is a high-pressure gas pipe for storing inert gas, and the pressure reducing valve 132 can release the inert gas through the intake manifold 31, and the compressor 131 and the four-way selector valve 133 can recover the inert gas through the return manifold 33, so as to realize the recycling of the inert gas;
[0117] The gas supply pipeline 134 on the four-way selection valve 133 can be used to supplement the inert gas when the content of the inert gas is insufficient. Of course, the reactor 1 is provided with a pressure relief valve to maintain the reaction pressure in the reactor 1 stable.
[0118] Based on the above embodiments, the negative pressure mechanism can reduce the pressure in the reaction kettle 1 to perform distillation, thereby obtaining polydimethylsiloxane photocurable slurry. Based on this, the following preferred embodiments are provided.
[0119] like Figure 2 As shown, the negative pressure mechanism includes a negative pressure pump 14 arranged on the reactor 1, and a negative pressure pipe 141 and a recovery pipe 142 are respectively arranged on the negative pressure pump 14. The negative pressure pipe 141 is connected with a vacuum distillation component 143, and the vacuum rectification component 143 is connected to the top of the reactor 1, and is used to change the vacuum degree of the reactor 1 and collect the distilled liquid. The recovery pipe 142 is connected to the return gas manifold 33 to recover or discharge the extracted inert gas.
[0120] Specifically, the vacuum distillation component 143 is a conventional component, which is equipped with a distillation pipeline with a cooling channel, a protection bottle, and a receiving bottle. The protection bottle is connected to the negative pressure pipe 141 to extract the pressure in the reactor 1. During this process, the steam flowing through the distillation pipeline is condensed into droplets and flows to the receiving bottle for collection;
[0121] The inert gas extracted from the negative pressure pipe 141 contains a certain amount of water vapor. After being connected to the recovery manifold 33, it is not recovered into the gas tank 13 by the compressor 131, but is discharged by the four-way selection valve 133 and the exhaust pipe 135 to avoid contaminating the inert gas in the gas tank 13.
[0122] Of course, the pressure relief valve can be directly connected to the return air manifold 33 through a pipeline, and the exhaust pipeline 135 can be connected to the exhaust gas treatment pipeline to discharge the inert gas containing a large amount of air discharged by the pressure relief valve (preliminarily replacing the air in the reactor 1 to achieve inert gas protection) to avoid direct discharge of inert gas.
[0123] Based on the preparation method of the composite photosensitive polymer material for photocurable 3D printing, a composite photosensitive polymer material for photocurable 3D printing is provided below. The composite photosensitive polymer material comprises: 50 to 80 parts of modified polydimethylsiloxane, 0.1 to 2 parts of photoinitiator, 1 to 8 parts of photosensitizer, 0.5 to 5 parts of dispersant, and 1 to 6 parts of thickener;
[0124] The modified polydimethylsiloxane is obtained by adding a silane coupling agent to polydimethylsiloxane under the protection of an inert gas and stirring at a temperature of 100 to 150° C. for 20 to 70 minutes;
[0125] The silane coupling agent is any one or more of an alkenyl group, a chloroalkyl group, an aminoalkyl group, a polysulfide alkyl group, an acryloyloxyalkyl group, and a cationic alkyl group, and the mass of the silane coupling agent accounts for 0.1-8% of the total mass of the polydimethylsiloxane;
[0126] Among them, the photoinitiator is any one of trimethylbenzoyl, methylphenylpropane, benzoyl formate, and hydroxycyclohexyl phenyl ketone, the photosensitizer is any one or more of azobenzene and distilbene photosensitive elements, the dispersant is any one or more of sodium polyacrylate, polyacrylate, and polyvinyl pyrrolidone, and the thickener is any one or more of methacrylic acid and acrylate.
[0127] In this embodiment, polydimethylsiloxane and silane coupling agent are stirred at a temperature of 100 to 150° C., a stirring speed of 250 to 680 rpm, and a stirring time of 20 to 70 min to perform surface modification of polydimethylsiloxane;
[0128] The chemical formula of polydimethylsiloxane is: (C2H6OSi)n. Polydimethylsiloxane has a regular and symmetrical structure, a small material polarity, and a hydrocarbon functional group at the end of the structural formula that is insoluble in water. It has good hydrophobicity, and polydimethylsiloxane is a powder with a diameter of 200nm to 1200nm.
[0129] The modified polydimethylsiloxane, the photoinitiator, the photosensitizer, the dispersant and the thickener are added to the reaction kettle for reaction, and the temperature is gradually increased in the range of 30-50°C at a rate of 2-10°C / min, and the mixture is continuously stirred to cause the reaction;
[0130] The mass of the photoinitiator accounts for 0.1-2% of the total mass of the photocurable slurry, the mass of the photosensitizer accounts for 5-20% of the total mass of the photocurable slurry, the mass of the dispersant accounts for 0.5-5% of the total mass of the photocurable slurry, and the mass of the thickener accounts for 1-6% of the total mass of the photocurable slurry.
[0131] Compared with existing photosensitive materials, the composite photosensitive polymer material in this embodiment is obtained by modifying polydimethylsiloxane and mixing it with a photoinitiator, a photosensitizer, a dispersant, and a thickener. It has good hydrophobicity, so when printing products with complex flow channels such as microfluidic chips, there is no need for secondary hydrophobic treatment.
[0132] Hydrophobicity and oleophobicity can be quantified by contact angle measurement. The larger the contact angle, the more hydrophobic and oleophobic the material surface is. The contact angle is determined by dropping a drop of water on the surface of the material and measuring the angle at which the water drop makes contact with the surface of the material. Generally, contact angles over 90° are considered hydrophobic, while those over 150° are considered super hydrophobic.
[0133] Specifically, polydimethylsiloxane (PDMS) is a polymer material with a silicon-oxygen bond as the main chain. This structure gives it excellent hydrophobic and oleophobic properties, extremely low surface tension, strong adhesion to other materials, and can be used for a long time in the range of -50 to 200°C.
[0134] Therefore, if polydimethylsiloxane (PDMS) is used as a photocurable material, after photocuring printing, it can produce good hydrophobic and oleophobic properties in the pores of the cured structure. However, polydimethylsiloxane is a non-photocurable material. Therefore, before it is processed into a photocurable material, it needs to be modified to enable it to have the ability to be photocured.
[0135] The commonly used photocurable material is usually epoxy acrylate resin, which contains ester groups, giving it certain hydrophobic and oleophobic properties. Its contact angle is approximately between 60° and 80°, and its hydrophobic and oleophobic properties are relatively weak. Microfluidic chips need to frequently complete liquid displacement experiments. Therefore, epoxy acrylate resin needs to be modified to obtain better hydrophobic and oleophobic properties. Even after modification, the contact angle is approximately between 90° and 120°.
[0136] However, polydimethylsiloxane achieves its excellent natural hydrophobic and oleophobic properties through the siloxane bonds (Si-O-Si) contained in its molecular chain. Its contact angle is approximately between 100° and 110°, and after modification, the contact angle is approximately between 120° and 150°, which can reach a super hydrophobic and oleophobic level. Therefore, using polydimethylsiloxane as the main raw material to make photocurable materials can make the molded body have excellent hydrophobic and oleophobic properties.
[0137] When the above-mentioned light-curing 3D printing composite photosensitive polymer material is used:
[0138] Place the polydimethylsiloxane photocurable slurry into the slurry tank of the photocurable 3D printer, and preheat and vibrate it through the pretreatment device in the printing tank to make the photocurable slurry fully and evenly mixed and have good fluidity, wherein the preheating temperature is 40-80°C, and the preheating and vibration are carried out simultaneously for 30-60 seconds;
[0139] The photocuring printer slurry nozzle uses a designed sensor to accurately control the flow of photocuring slurry to ensure the consistency of the single layer thickness of a single product;
[0140] The 3D printer performs light curing according to the thickness of each layer of 30-100μm, the UV light intensity is maintained at 5-15mW / cm2, and the exposure time of each layer is ≤30s;
[0141] After printing, the product is transferred to the cleaning device via an automatic conveyor belt, where it is cleaned with a solvent to remove excess photocurable slurry and dried;
[0142] After being transferred to the 360° ultraviolet light irradiation area, the product is cured by irradiation for 15 to 60 seconds.
[0143] The above embodiments are only exemplary embodiments of the present application and are not intended to limit the present application. The protection scope of the present application is defined by the claims. Those skilled in the art may make various modifications or equivalent substitutions to the present application within the essence and protection scope of the present application, and such modifications or equivalent substitutions shall also be deemed to fall within the protection scope of the present application.
Claims
1. A method for preparing a composite photosensitive polymer material for photocuring 3D printing, characterized in that: The steps include: Step 100, preheating the reaction kettle with inert gas and placing a certain amount of polydimethylsiloxane into the reaction kettle, heating it to a preset temperature with inert gas and stirring it, and at the same time, spraying a certain amount of silane coupling agent into the reaction kettle to obtain modified polydimethylsiloxane after stirring for a preset time; Step 200, after the modified polydimethylsiloxane in the reactor is stirred and cooled to a preset value by using an inert gas, a certain amount of photoinitiator, photosensitizer, dispersant, and thickener are added to the reactor and stirred, and at the same time, stirred at a set temperature rise rate to obtain a mixed solution after stirring for a preset time; Step 300, using an inert gas to cool the mixed solution in the reactor to a preset value, and using a vacuum distiller to adjust the pressure in the reactor to a preset negative pressure value, distilling the mixed solution in the reactor, and cooling it to room temperature after the distillation reaches a preset time, so as to discharge and filter to obtain polydimethylsiloxane photocuring slurry.
2. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1, characterized in that: In step 100, the gas-preserved heat stirring treatment method for stirring and modifying polydimethylsiloxane and a silane coupling agent includes: Inert gas is transported into the reactor through pipelines so that the reactor is filled with inert gas to form gas protection, and hot inert gas is introduced into the hollow stirring blades in the reactor so that the temperature of the stirring blades is raised to a set temperature; A fixed amount of polydimethylsiloxane and a silane coupling agent are sequentially added to the feeder on the reactor, and the polydimethylsiloxane and the silane coupling agent enter the pipeline from the feeder, and are carried by the airflow transported into the reactor and sprayed into the reactor; The polydimethylsiloxane and silane coupling agent sprayed into the reaction kettle are in an environment protected by inert gas, and the polydimethylsiloxane and silane coupling agent are stirred by stirring blades after entering the reaction kettle; At the same time, the stirring blade heated by the hot inert gas quickly heats the polydimethylsiloxane and the silane coupling agent to reach the set reaction temperature and continues stirring until the set time ends to obtain modified polydimethylsiloxane.
3. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1, characterized in that: In step 200, the gas-heated stirring treatment method for stirring and mixing the modified polydimethylsiloxane with the photoinitiator, the photosensitizer, the dispersant, and the thickener includes: After the polydimethylsiloxane modification is completed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and stirring is continued for a certain period of time so that the temperature of the modified polydimethylsiloxane reaches the same temperature as that of the stirring blade; Continue to add a certain amount of photoinitiator, photosensitizer, dispersant and thickener to the feeder on the reactor in sequence, and the photoinitiator, photosensitizer, dispersant and thickener enter the pipeline from the feeder in sequence, and are carried by the airflow transported into the reactor and sprayed into the reactor; The photoinitiator, photosensitizer, dispersant and thickener sprayed into the reaction kettle are in an environment protected by inert gas, and the photoinitiator, photosensitizer, dispersant and thickener are stirred by stirring blades after entering the reaction kettle; At the same time, the inert gas introduced into the stirring blade gradually heats up at a set temperature rise rate, and stirs and heats the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant, and thickener until the set stirring time ends to obtain a mixed solution.
4. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1, characterized in that: In step 300, the method for implementing the reduced pressure distillation reaction of the mixed solution includes: After the modified polydimethylsiloxane and the photoinitiator, photosensitizer, dispersant and thickener are uniformly mixed in the reactor, the temperature of the inert gas introduced into the stirring blade is reduced to a preset temperature and the stirring is continued for a certain period of time so that the temperature of the mixed solution reaches the same temperature as the stirring blade; The negative pressure distiller on the reactor is used to evacuate the interior of the reactor to make the pressure inside the reactor reach the set pressure value, and the temperature and pressure state in the reactor are maintained for a set time. At the same time, the stirring blade rotates slowly to stir the mixed solution in the reactor for a set time; After the reduced pressure distillation reaches the set time, the temperature of the inert gas introduced into the stirring blade is reduced to the preset temperature and stirring is continued for a certain period of time to reduce the temperature of the mixed solution to room temperature, and the product is discharged from the reactor and filtered to obtain polydimethylsiloxane photocuring slurry.
5. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1 or 2, characterized in that: In step 100, the polydimethylsiloxane modification stirring reaction temperature is 100-150° C., the stirring speed is 250-680 rpm, and the stirring time is 20-70 min.
6. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1 or 3, characterized in that: In step 200, the basic reaction temperature of the modified polydimethylsiloxane with the photoinitiator, photosensitizer, dispersant and thickener is 30-50°C, the stirring heating rate is 2-10°C / min, and the stirring time is 5-30min.
7. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 1 or 4, characterized in that: In step 300, the mixed solution is subjected to reduced pressure distillation in a reactor with a vacuum degree of 0.01 to 20 kPa and a reaction time of 1 to 10 hours. After the reaction is completed, the product inside the reactor is cooled to room temperature.
8. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to any one of claims 1 to 4, characterized in that: The reaction device for stirring and modifying polydimethylsiloxane and silane coupling agent, stirring and mixing modified polydimethylsiloxane with photoinitiator, photosensitizer, dispersant and thickener, and distilling the mixed solution under reduced pressure comprises: A reactor, wherein a protection pipeline is provided on the reactor for conveying inert gas protection into the reactor; Two stirring shafts are symmetrically arranged in the reactor and rotate synchronously; A temperature regulating pipeline, partly arranged in the two stirring shafts, the temperature regulating pipeline comprises an intake manifold, two stirring pipelines, and a return manifold which are rotatably connected in sequence, the intake manifold and the return manifold are respectively arranged at both ends of the two stirring shafts and fixed outside the reactor, the two stirring pipelines are arranged in the stirring shafts and partially exposed in the reactor, and the part of the stirring pipeline exposed in the reactor extends outward to form a stirring blade arranged around the stirring shaft; A feeder, arranged on the reactor and connected to the protection pipeline, used to feed the reaction material into the protection pipeline and spray it into the reactor along with the inert gas flow; A negative pressure mechanism, arranged on the reactor and connected to the temperature regulating pipeline, is used to extract gas from the reactor to generate negative pressure and return the extracted inert gas to the temperature regulating pipeline; When stirring reaction is required, after the stirring shaft rotates the stirring pipeline to stir, the protection pipeline is opened to introduce inert gas protection and hot gas is introduced into the temperature control pipeline to heat the stirring pipeline. At the same time, a quantitative reaction material is added to the reactor through the feeder and the protection pipeline, and then the protection pipeline is closed, and the negative pressure mechanism adjusts the pressure in the reactor according to the reaction requirements to continuously stir for a preset time to obtain the target product.
9. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 8, characterized in that: The stirring pipeline includes a plurality of junction boxes, and a plurality of blade tubes distributed around the axis of each of the adjacent junction boxes are arranged to communicate with each other, and the axially adjacent blade tubes are arranged in an annular pattern, and the blade tubes are fixed on the stirring shaft in a U shape; The stirring shaft is provided with a plurality of chambers, the plurality of chambers are used to fix a plurality of junction boxes, a plurality of fixing holes are provided on the side wall of the stirring shaft, each of the fixing holes is connected to the corresponding chamber, and the blade tube extends out of the stirring shaft through the fixing hole and is fixed; Both ends of the stirring shaft are provided with rotating holes, and the two rotating holes are respectively connected to the two chambers on the outside. The branch ends of the intake manifold and the return manifold are sealed and rotatably inserted into the rotating holes and are respectively rotatably connected to the two junction boxes on the outside.
10. The method for preparing a composite photosensitive polymer material for photocuring 3D printing according to claim 9, characterized in that: The feeder comprises two feeding hoppers with sealing covers, the bottoms of the two feeding hoppers are connected with feeding manifolds, and the feeding manifolds are connected with the protection pipeline to add solid materials and liquid materials into the protection pipeline respectively; The protection pipeline is provided with two boosting pipelines through a one-way valve, and the two boosting pipelines are respectively provided on the two feeding hoppers, so as to introduce inert gas into the feeding hopper for boosting the pressure when adding materials; The negative pressure mechanism includes a negative pressure pump arranged on the reactor, and the negative pressure pump is respectively provided with a negative pressure pipe and a recovery pipe, the negative pressure pipe is connected with a vacuum distillation component, and the vacuum rectification component is connected to the top of the reactor, which is used to change the vacuum degree of the reactor and collect the distilled liquid, and the recovery pipe is connected to the return gas manifold to recover or discharge the extracted inert gas.