A method and system for preparing flame-retardant unsaturated polyester resin

By using a three-reactor system and precise temperature control, the problem of inaccurate temperature control in the preparation of unsaturated polyester resin was solved, thereby improving the quality and heat resistance of the resin.

CN118059521BActive Publication Date: 2026-03-06西安新三力复合材料科技有限公司
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Patent Information

Application Number
CN202410206438.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-02-26
Publication Date
2026-03-06
Estimated Expiration
2044-02-26

AI Technical Summary

Technical Problem

In the existing technology, the temperature control is not precise during the preparation of unsaturated polyester resin, resulting in poor resin quality and affecting the performance of flame-retardant unsaturated polyester resin.

Method used

A three-reactor system is adopted, which combines temperature control components and a cooling system. The temperature of the reactor is precisely controlled through a heat transfer oil tank, temperature sensor and heating components to ensure that the temperature is within the required range and to avoid viscosity increase or gelation.

Benefits of technology

High-quality preparation of unsaturated polyester resin was achieved, significantly improving its heat resistance.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

This invention discloses a flame-retardant unsaturated polyester resin preparation system and method, belonging to the field of polyester resin technology. It includes: a reaction vessel for preparing a flame retardant and an unsaturated polyester resin, and a temperature control system for controlling the temperature of the first, second, and third reaction vessels during operation. Through the configured first, second, and third temperature control components and cooling system, the temperature at different stages of operation in the first, second, and third reaction vessels can be precisely controlled, ensuring that the reaction proceeds according to the process. This avoids problems such as increased viscosity and high acid value of the unsaturated polyester resin due to inaccurate temperature control, or resin gelation, thus ensuring higher quality flame-retardant unsaturated polyester resin and significantly improving the heat resistance of the unsaturated polyester resin.
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Description

Technical Field

[0001] This invention relates to the field of polyester resin technology, and specifically to a method and system for preparing flame-retardant unsaturated polyester resin. Background Technology

[0002] Unsaturated polyester resin (UPR) is a linear polymer compound formed by the condensation of diol and unsaturated dicarboxylic acid (anhydride). In order to improve the heat resistance of unsaturated polyester resin, for example, the prior art, Chinese invention patent application number: CN202210584402.5, discloses a method for preparing flame-retardant unsaturated polyester resin, which involves first synthesizing a flame retardant, then synthesizing an unsaturated polyester resin, and finally mixing the two substances to form a flame-retardant unsaturated polyester resin.

[0003] In the actual preparation process, temperature has a great influence on unsaturated polyester resin. Too rapid heating will lead to the loss of propylene glycol, which will increase the viscosity and acid value. Too high a temperature will easily cause the resin to gel. Overall, temperature control is crucial to the performance of unsaturated polyester resin. In the above-disclosed method for preparing unsaturated polyester resin, the temperature control is not precise, which leads to the low quality of the unsaturated polyester resin and ultimately affects the performance of the flame-retardant unsaturated polyester resin. Summary of the Invention

[0004] To address the problems of existing technologies, this invention provides a method and system for preparing flame-retardant unsaturated polyester resin.

[0005] On one hand, the present invention provides a flame-retardant unsaturated polyester resin preparation system, comprising:

[0006] The first reaction vessel is used to prepare flame retardants;

[0007] The second reaction vessel is used to prepare unsaturated polyester resin;

[0008] The third reaction vessel is used to mix flame retardants and unsaturated polyester resin to prepare flame-retardant unsaturated polyester resin.

[0009] Temperature control system, used for temperature control during the operation of the first reactor, second reactor and third reactor;

[0010] The temperature control system includes: a heating system and a cooling system;

[0011] The heating system includes: a heat transfer oil tank and a temperature control component connected to the heat transfer oil tank pipeline;

[0012] The heat transfer oil tank is equipped with a temperature sensor and a heating component for heating the heat transfer oil.

[0013] The temperature control assembly includes: a first temperature control assembly, a second temperature control assembly, and a third temperature control assembly, which are respectively connected to the first reaction vessel, the second reaction vessel, and the third reaction vessel;

[0014] The first temperature control component, the second temperature control component, and the third temperature control component are also connected to the cooling system and the heat transfer oil tank pipeline, respectively;

[0015] The heat transfer oil tank has a first output end and a second output end. The first output end is connected to an oil pump, and the oil pump is connected to the first temperature control component, the second temperature control component and the third temperature control component respectively.

[0016] The first, second, and third temperature control components are used to compensate for the temperature of the heat transfer oil during the operation of the first, second, and third reaction vessels, respectively, so that the temperature of the heat transfer oil is controlled within the required range; the cooling system is used to cool the heat transfer oil in the heat transfer oil tank before supplying it to the first, second, and third reaction vessels; during the temperature regulation process, the operation of each component is controlled by an external computer.

[0017] Furthermore, the outer sides of the first, second, and third reaction vessels are all provided with heat-insulating shells, and the heat-insulating shells have a sealed cavity structure.

[0018] Each of the insulation shells is equipped with a spiral tube. One end of the spiral tube passes through the insulation shell and is connected to the output terminals of the first temperature control component, the second temperature control component, and the third temperature control component, respectively. The other end of the spiral tube passes through the insulation shell and is connected to the heat transfer oil tank.

[0019] Furthermore, the first temperature control component includes: a first temperature transmitter, a second temperature transmitter, a first heating chamber, a first remote control valve, a second remote control valve, and a third remote control valve;

[0020] The output end of the oil pump is provided with a flow divider pipe, and the output end of the flow divider pipe is provided with three branches, namely the first branch, the second branch and the third branch, which are respectively connected to the first temperature control component, the second temperature control component and the third temperature control component;

[0021] The first branch includes: a first oil pipe and a first return assembly;

[0022] One end of the first oil pipe is connected to the diversion pipe, and the other end of the first oil pipe is connected to one end of the spiral tube on the first reactor.

[0023] The first temperature transmitter and the first remote control valve are sequentially installed on the first oil pipe, with the first temperature transmitter located close to the shunt pipe.

[0024] The first reflux assembly includes: a first pipe, a second pipe, and a third pipe;

[0025] One end of the first pipe is connected to the first oil pipe between the first temperature transmitter and the first remote control valve, and the other end of the first pipe is connected to the input end of the first heating box.

[0026] One end of the second pipe is connected to the output end of the first heating box, and the other end of the second pipe is connected to the first oil pipe between the first remote control valve and the first reaction vessel;

[0027] One end of the third pipe is connected to the second pipe, and the other end of the third pipe is connected to the top of the first heating box;

[0028] The third remote control valve is installed on the first pipeline, the second temperature transmitter and the second remote control valve are both installed on the second pipeline, the second remote control valve is located on the second pipeline between the third pipeline and the first oil pipe, and the second temperature transmitter is located on the second pipeline between the second remote control valve and the first heating box.

[0029] Furthermore, the second temperature control component includes: a third temperature transmitter, a fourth temperature transmitter, a second heating chamber, a fourth remote control valve, a fifth remote control valve, and a sixth remote control valve;

[0030] The second branch includes: a second oil pipe and a second return assembly;

[0031] One end of the second oil pipe is connected to the diversion pipe, and the other end of the second oil pipe is connected to one end of the spiral tube on the second reactor.

[0032] The third temperature transmitter and the fourth remote control valve are sequentially installed on the second oil pipe, and the third temperature transmission is located near the splitter pipe;

[0033] The second return pipe includes: a fourth pipe, a fifth pipe, and a sixth pipe;

[0034] One end of the fourth pipe is connected to the second oil pipe between the third temperature transmitter and the fourth remote control valve, and the other end of the fourth pipe is connected to the input end of the second heating box.

[0035] One end of the fifth pipe is connected to the output end of the second heating box, and the other end of the fifth pipe is connected to the second oil pipe between the fourth remote control valve and the second reaction vessel;

[0036] One end of the sixth pipe is connected to the fifth pipe, and the other end of the sixth pipe is connected to the top of the second heating box;

[0037] The sixth remote control valve is installed on the fourth pipe, the fourth temperature transmitter and the fifth remote control valve are both installed on the fifth pipe, the fifth remote control valve is located on the fifth pipe between the sixth pipe and the second oil pipe, and the fourth temperature transmitter is located on the fifth pipe between the fifth remote control valve and the second heating box.

[0038] Furthermore, the third temperature control component includes: a fifth temperature transmitter, a sixth temperature transmitter, a third heating chamber, a seventh remote control valve, an eighth remote control valve, and a ninth remote control valve;

[0039] The third branch includes: a third oil pipe and a third return assembly;

[0040] One end of the third oil pipe is connected to the diversion pipe, and the other end of the third oil pipe is connected to one end of the spiral tube on the third reactor.

[0041] The fifth temperature transmitter and the seventh remote control valve are sequentially installed on the third oil pipe, with the fifth temperature transmitter located close to the shunt pipe;

[0042] The third reflux assembly includes: a seventh pipe, an eighth pipe, and a ninth pipe;

[0043] One end of the seventh pipe is connected to the third oil pipe between the fifth temperature transmitter and the seventh remote control valve, and the other end of the seventh pipe is connected to the input end of the third heating box.

[0044] One end of the eighth pipe is connected to the output end of the third heating box, and the other end of the eighth pipe is connected to the third oil pipe between the seventh remote control valve and the third reaction vessel;

[0045] One end of the ninth pipe is connected to the eighth pipe, and the other end of the ninth pipe is connected to the top of the third heating box;

[0046] The ninth remote control valve is installed on the seventh pipe, and the sixth temperature transmitter and the eighth remote control valve are both installed on the eighth pipe. The eighth remote control valve is located on the eighth pipe between the ninth pipe and the third oil pipe, and the sixth temperature transmitter is located on the eighth pipe between the eighth remote control valve and the third heating box.

[0047] Furthermore, the input end of the heat transfer oil tank is provided with an oil return pipe;

[0048] The other ends of the spiral tubes on the first, second, and third reactors are respectively connected to the return oil pipe through the first, second, and third loop pipes; the first, second, and third loop pipes are respectively equipped with a tenth remote control valve, an eleventh remote control valve, and a twelfth remote control valve; the return oil pipe is equipped with an eighth temperature transmitter and a thirteenth remote control valve; the thirteenth remote control valve is located near the input end of the heat transfer oil tank.

[0049] Furthermore, the cooling system includes: a liquid cooling component, a gas cooling component, and an insulation box;

[0050] The liquid cooling assembly includes: a liquid storage tank, a first delivery pump, and a first bend in the pipe;

[0051] The storage tank contains coolant, and the input and output ends of the first delivery pump are respectively connected to the pipelines on both sides of the storage tank.

[0052] The first bend is located on the pipeline between the output end of the first delivery pump and the liquid storage tank;

[0053] The gas cooling assembly includes: a cold medium tank, a second delivery pump, and a second bend in the pipe;

[0054] The refrigerant tank contains refrigerant, and the input and output ends of the second delivery pump are respectively connected to the pipelines on both sides of the refrigerant tank.

[0055] The second bend is located on the pipeline between the output end of the second delivery pump and the refrigerant tank;

[0056] The second output end of the heat transfer oil tank is connected to the cooling pipe through a pipeline. The cooling pipe is located between the first bend and the second bend, and is in close contact with the first bend and the second bend.

[0057] The first bend, the second bend, and the cooling pipe are installed inside the insulation box; the end of the cooling pipe is connected to the pipeline between the heat transfer oil tank and the oil pump through a pipe, and a seventh temperature transmitter is installed on the pipe. The seventh temperature transmitter is located close to the insulation box. A branch pipe is installed between the pipeline and the heat transfer oil tank, and a sixteenth remote control valve is installed on the branch pipe.

[0058] A fourteenth remote control valve is installed on the pipeline between the heat transfer oil tank and the oil pump; a fifteenth remote control valve is installed on the pipeline between the cooling pipe and the heat transfer oil tank; and a seventeenth remote control valve is installed on the pipeline between the cooling pipe and the oil pump.

[0059] Furthermore, the first and second bends are spiral or wavy, and the shape of the cooling pipe is adapted to the shape of the first and second bends.

[0060] Furthermore, the heat transfer oil tank is equipped with an oil diffusion component, which is used to disperse the heat transfer oil input into the heat transfer oil tank from the oil supply station to form an oil mist;

[0061] The oil diffusion assembly includes: a motor and a rotor;

[0062] The motor is connected to the outer surface of the heat transfer oil tank, the output end of the motor is connected to a rotating shaft, the rotating shaft is located inside the heat transfer oil tank, the rotating wheel is connected to the rotating shaft, and the surface of the rotating shaft is provided with several blades in the vertical direction;

[0063] The heating components inside the heat transfer oil tank include: a heating plate and a heating block;

[0064] The heating block includes several arc-shaped plates connected in sequence, the diameter of the arc-shaped plates increases sequentially, and the bottom of the arc-shaped plates are located on the same plane;

[0065] The heating plate is located below the rotating wheel. The front and rear sides and the left side of the heating plate are sealed to the front and rear side walls and the left side wall of the heat transfer oil tank, respectively. A gap is left between the right side of the heating plate and the right side wall of the heat transfer oil tank.

[0066] The heating blocks are provided in multiple ways and are connected in sequence to form a staircase-like structure. The heating blocks near the right side of the heat transfer oil tank are higher than the heating blocks near the left side of the heat transfer oil tank.

[0067] The heating block is located below the heating plate. The right side and front and rear sides of the heating block are sealed to the right side and front and rear side walls of the heat transfer oil tank, respectively. A gap is left between the left side of the heating block and the left side wall of the heat transfer oil tank.

[0068] When the heat transfer oil is injected at high speed into the heat transfer oil tank, the heat transfer oil comes into contact with the front of the rotating wheel. The rotating wheel disperses the heat transfer oil into an oil mist, which then falls onto the heating plate. The heating plate heats the heat transfer oil. As the amount of heat transfer oil increases, the heat transfer oil gradually flows to the right side of the heating plate, then falls from the right side of the heating plate onto the heating block, and finally flows to the bottom of the heat transfer oil and is pumped away by the oil pump.

[0069] Furthermore, the heat transfer oil tank is provided with a first support plate and a second support plate;

[0070] The first support plate and the second support plate are disposed between the heating block and the heating plate. The left side of the first support plate is connected to the left inner wall of the heat transfer oil tank through a first rotating shaft. A groove is provided on the inner wall of the heat transfer oil tank, and the rotating shaft is rotatably connected in the groove.

[0071] The left side of the first support plate is connected to the rotating shaft, and the top of the first support plate is connected to the heating plate. The first support plate is provided with a through hole that corresponds to the position of the protrusion on the heating plate, and the lower end of the protrusion passes through the corresponding through hole.

[0072] The second support plate is located below the first support plate, and the first support plate and the second support plate are connected by a first connecting plate and a second connecting plate.

[0073] An electric telescopic rod is provided on the top of the heat transfer oil tank. The moving part of the electric telescopic rod is located inside the heat transfer oil tank and is rotatably connected to the right side of the first support through a first ring. When the computer controls the electric telescopic rod to move, the first support plate tilts.

[0074] A motor is provided on the outer left side of the heat transfer oil tank. A second rotating shaft is provided at the output end of the motor. One end of the second rotating shaft is located inside the heat transfer oil tank. A second ring is provided at the end of the second rotating shaft, which is located inside the heat transfer oil tank.

[0075] A third rotating shaft is provided between the first connecting plate and the second connecting plate. One end of the third rotating shaft passes through the first connecting plate and is rotatably connected to the second ring through the third ring. The other end of the third rotating shaft is rotatably connected to the second connecting plate.

[0076] The third rotating shaft is provided with a number of cams adapted to the position of the protrusion. The cams contact the corresponding protrusions respectively. When the computer controls the motor to operate, the second rotating shaft and the third rotating shaft rotate, synchronously driving the cams to rotate. At the same time, the protrusions perform vertical extension and retraction movements on the corresponding arc plate.

[0077] On the other hand, this application provides a method for preparing a flame-retardant unsaturated polyester resin, wherein the preparation method is applied in the above-mentioned preparation system and includes:

[0078] To prepare the flame retardant, a catalyst is added to the first reactor under nitrogen protection. A temperature sensor monitors the oil temperature in real time. If the oil temperature is below a set range, the computer controls the heating element to heat the heat transfer oil. The temperature in the heat transfer oil tank is monitored in real time by the temperature sensor until the oil temperature rises to within the set range. Then, the oil pump delivers the heat transfer oil to the first oil pipe. The first temperature transmitter monitors the oil temperature. If the oil temperature is within the set range, it directly enters the spiral tube on the first reactor. If the oil temperature is lost during delivery and falls below the set range... If the temperature is within the set range, the heat transfer oil is controlled to enter the first heating box for heating to compensate for the oil temperature. Then, the oil temperature is detected by the second temperature transmitter until the oil temperature reaches the set range value. Then, the heat transfer oil is controlled to enter the spiral tube on the first reactor. Then, the stirrer is controlled to stir the added material and the solenoid valve on the trimethyl phosphite storage tank is controlled to open, and trimethyl phosphite is added dropwise to the first reactor. After the dropwise addition is completed, the temperature is heated to reflux and reacted at atmospheric pressure for 5 to 6 hours. The fraction with a temperature of 97 to 1-5℃ / 5KPa is collected by vacuum distillation, which is dimethyl methylphosphonate.

[0079] To prepare unsaturated polyester resin, under nitrogen protection, isophthalic acid, fumaric acid, pentaerythritol, D-33 diol, and a modified molecular sieve catalyst are first added to the second reactor. After addition, nitrogen is continuously purged. A temperature sensor monitors the oil temperature in real time. If the oil temperature is lower than the set range, the computer controls the heating element to heat the heat transfer oil. The temperature in the heat transfer oil tank is monitored in real time by the temperature sensor until the oil temperature rises to within the set range. Then, the oil pump delivers the heat transfer oil to the second oil pipe, and a third temperature transmitter monitors the oil temperature. If the oil temperature is within the set range, it directly enters the spiral tube on the second reactor. If the oil temperature is lost during transportation and falls below the set range, the heat transfer oil is controlled to enter the second heating box to compensate for the oil temperature. Then, the oil temperature is detected by the fourth temperature transmitter until the oil temperature returns to the set range. Then, the heat transfer oil is controlled to enter the spiral tube on the second reactor, and the stirrer on the second reactor is controlled to stir the added material. The heating temperature is 165-185℃, the heating rate is 12-15℃ / h, and the reaction continues for 25-35 minutes. Then, the temperature is further increased to 245-260℃, the heating rate is 2-3℃ / h, and the stirring lasts for 2.5-3 hours to obtain the unsaturated polyester resin solution.

[0080] Synthesis of flame-retardant unsaturated resin: Dimethyl methylphosphonate, anhydrous ethanol, aluminum oxide, and sodium hydroxide solution were added to a third reaction vessel for dissolution, and the prepared unsaturated polyester resin was added. The temperature was then raised to 40-45°C under computer control, and the reaction was stirred for 3.5-4.5 hours. The temperature was then raised to 85-90°C, and saturated potassium carbonate solution was added. After stirring for 3.5-4.5 hours, diaminosilane was added dropwise, and diethylene glycol acetate was continuously added to maintain a certain fluidity of the material. After rotary evaporation of the solvent, the product was washed until neutral and dried to obtain the flame-retardant unsaturated polyester resin.

[0081] The beneficial effects of this invention are:

[0082] This invention provides a flame-retardant unsaturated polyester resin preparation system and method. By setting up a first temperature control component, a second temperature control component, a third temperature control component, and a cooling system, the temperature at different stages of operation of the first, second, and third reaction vessels can be precisely controlled, thereby ensuring that the reaction proceeds according to the process. This avoids the problems of increased viscosity and high acid value of the unsaturated polyester resin or resin gelation caused by inaccurate temperature control, thus ensuring higher quality flame-retardant unsaturated polyester resin and significantly improving the heat resistance of the unsaturated polyester resin. Attached Figure Description

[0083] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0084] Figure 1 This is a schematic diagram of the overall structure provided by the present invention;

[0085] Figure 2 This is a schematic diagram of the flow direction of the heat transfer oil in the heat transfer oil tank provided by the present invention;

[0086] Figure 3 This is a schematic diagram of the heating plate structure provided by the present invention.

[0087] Figure reference numerals: 1 is the first reactor, 2 is the second reactor, 3 is the third reactor, 4 is the heat transfer oil tank, 5 is the insulation shell, 6 is a temperature transmitter, 7 is a second temperature transmitter, 8 is the first heating box, 9 is the first remote control valve, 10 is the second remote control valve, 11 is the third remote control valve, 12 is the oil pump, 13 is the first oil pipe, 14 is the first pipeline, 15 is the second pipeline, 16 is the third pipeline, 17 is the third temperature transmitter, 18 is the fourth temperature transmitter, 19 is the second heating box. The heating chamber is connected to the following pipes: 20 is the fourth remote control valve, 21 is the fifth remote control valve, 22 is the sixth remote control valve, 23 is the second oil pipe, 24 is the fourth pipeline, 25 is the fifth pipeline, 26 is the fifth temperature transmitter, 27 is the sixth temperature transmitter, 28 is the third heating chamber, 29 is the seventh remote control valve, 30 is the eighth remote control valve, 31 is the ninth remote control valve, 32 is the third oil pipe, 33 is the seventh pipeline, 34 is the eighth pipeline, 35 is the ninth pipeline, 36 is the first circuit pipe, and 37 is the second circuit pipe. 38 is the third loop pipe, 39 is the tenth remote control valve, 40 is the eleventh remote control valve, 41 is the twelfth remote control valve, 42 is the eighth temperature transmitter, 43 is the thirteenth remote control valve, 44 is the liquid storage tank, 45 is the first transfer pump, 46 is the first bend, 47 is the refrigerant tank, 48 is the second transfer pump, 49 is the second bend, 50 is the cooling pipe, 51 is the insulation box, 52 is the seventh temperature transmitter, 53 is the sixteenth remote control valve, 54 is the fourteenth remote control valve, and 55 is the tenth... 56 is the seventeenth remote control valve, 57 is the heating plate, 58 is the sixth pipe, 59 is the rotating wheel, 60 is the rotating shaft, 61 is the blade, 62 is the heating block, 63 is the first support plate, 64 is the second support plate, 65 is the first connecting plate, 66 is the second connecting plate, 67 is the first rotating shaft, 68 is the third rotating shaft, 69 is the second rotating shaft, 70 is the second ring, 71 is the third ring, 72 is the cam, 73 is the first ring, 74 is the electric telescopic rod, and 75 is the motor. Detailed Implementation

[0088] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0089] Example 1

[0090] See Figures 1 to 3 A flame-retardant unsaturated polyester resin preparation system, comprising:

[0091] First reaction vessel 1, used for preparing flame retardants;

[0092] The second reaction vessel 2 is used to prepare unsaturated polyester resin;

[0093] The third reaction vessel 3 is used to mix flame retardant and unsaturated polyester resin to prepare flame retardant unsaturated polyester resin.

[0094] The first reactor 1, the second reactor 2 and the third reactor 3 are all provided with heat insulation shells 5 on their outer sides, and the heat insulation shells 5 are in the form of a closed cavity structure.

[0095] Each of the heat insulation shells 5 is provided with a spiral tube. One end of the spiral tube passes through the heat insulation shell 5 and is connected to the output terminals of the first temperature control component, the second temperature control component, and the third temperature control component respectively. The other end of the spiral tube passes through the heat insulation shell 5 and is connected to the heat transfer oil tank 4. The heat insulation shell is filled with a ceramic plate, which is located between the spiral tube and the inner wall of the heat insulation shell.

[0096] A temperature control system is used to control the temperature of the first reactor 1, the second reactor 2, and the third reactor 3 during operation.

[0097] The temperature control system includes: a heating system and a cooling system;

[0098] The heating system includes: a heat transfer oil tank 4 and a temperature control component connected to the heat transfer oil tank 4 via pipeline;

[0099] The heat transfer oil tank 4 is equipped with a temperature sensor and a heating component for heating the heat transfer oil.

[0100] The temperature control assembly includes: a first temperature control assembly, a second temperature control assembly, and a third temperature control assembly, which are respectively connected to the first reactor 1, the second reactor 2, and the third reactor 3;

[0101] The first temperature control component, the second temperature control component, and the third temperature control component are also respectively connected to the cooling system and the heat transfer oil tank 4 pipeline;

[0102] The heat transfer oil tank 4 has a first output end and a second output end. The first output end is connected to an oil pump 12, which is connected to the first temperature control component, the second temperature control component and the third temperature control component respectively.

[0103] The first, second, and third temperature control components are used to compensate for the temperature of the heat transfer oil during the operation of the first reactor 1, the second reactor 2, and the third reactor 3, respectively, so that the temperature of the heat transfer oil is controlled within the required range; the cooling system is used to cool the heat transfer oil in the heat transfer oil tank 4 before supplying it to the first reactor 1, the second reactor 2, and the third reactor 3; during the temperature regulation process, the operation of each component is controlled by an external computer.

[0104] The cooling system is mainly used when the temperature drops significantly at different stages of the reactor's operation. Significant cooling relying on self-heating is time-consuming, and the reaction process is still ongoing. Therefore, when significant cooling is required at different stages of the reactor's operation, the cooling system can be set up to quickly reduce the temperature to the required level.

[0105] The cooling system includes: a liquid cooling component, a gas cooling component, and an insulation box 51;

[0106] The liquid cooling assembly includes: a liquid storage tank 44, a first delivery pump 45, and a first bend 46;

[0107] The storage tank 44 is filled with coolant, and the input and output ends of the first delivery pump 45 are respectively connected to the pipelines on both sides of the storage tank 44.

[0108] The first bend 46 is disposed on the pipeline between the output end of the first delivery pump 45 and the liquid storage tank 44;

[0109] The air cooling assembly includes: a cold medium tank 47, a second delivery pump 48, and a second bend 49;

[0110] The refrigerant tank 47 contains refrigerant, and the input and output ends of the second delivery pump 48 are respectively connected to the pipelines on both sides of the refrigerant tank 47.

[0111] The second bend 49 is disposed on the pipeline between the output end of the second delivery pump 48 and the refrigerant tank 47;

[0112] The second output end of the heat transfer oil tank 4 is connected to the cooling pipe 50 through a pipeline. The cooling pipe 50 is disposed between the first bend 46 and the second bend 49, and the cooling pipe 50 is in close contact with the first bend 46 and the second bend 49.

[0113] The first bend 46, the second bend 49, and the cooling pipe 50 are disposed inside the insulation box 51; the end of the cooling pipe 50 is connected to the pipeline between the heat transfer oil tank 4 and the oil pump 12 through a pipe, and a seventh temperature transmitter 52 is disposed on the pipeline. The seventh temperature transmitter 52 is disposed close to the insulation box 51. A branch pipe is disposed between the pipeline and the heat transfer oil tank 4, and a sixteenth remote control valve 53 is disposed on the branch pipe.

[0114] A fourteenth remote control valve 54 is installed on the pipeline between the heat transfer oil tank 4 and the oil pump 12; a fifteenth remote control valve 55 is installed on the pipeline between the cooling pipe 50 and the heat transfer oil tank 4; and a seventeenth remote control valve 56 is installed on the pipeline between the cooling pipe 50 and the oil pump.

[0115] The first and second bends are spiral or wavy, and the shape of the cooling pipe is adapted to the shape of the first and second bends.

[0116] When the reactor experiences a significant temperature drop during operation, the heat transfer oil returns to the heat transfer oil tank. The fourteenth and seventeenth remote control valves are then closed, while the fifteenth and sixteenth remote control valves are opened. The heat transfer oil enters the cooling pipe. At this time, the first and second delivery pumps operate, causing coolant and cold medium to flow in the first and second bends respectively, exchanging heat with the heat transfer oil. When the heat transfer oil flows through the seventh temperature transmitter, if the measured oil temperature is not within the set range, it flows back to the heat transfer oil tank. This process continues until the temperature reaches the set range. Then, the sixteenth and fourteenth remote control valves are closed, the seventeenth remote control valve is opened, and the oil pump is started to deliver the heat transfer oil into the corresponding temperature control component.

[0117] When the heat transfer oil flows to the cooling pipe, it is achieved by a power pump (not shown in the figure). The power pump is installed in the insulation box. The input end of the power pump is connected to the pipeline port between the insulation box and the heat transfer oil box, and the output end of the power pump is connected to the input port of the cooling pipe.

[0118] In order to improve the heating effect of the heat transfer oil, an oil diffusion component is installed in the heat transfer oil tank 4 to disperse the heat transfer oil input into the heat transfer oil tank from the oil supply station and form an oil mist.

[0119] The oil diffusion assembly includes: a motor and a rotor 59;

[0120] The motor is connected to the outer surface of the heat transfer oil tank 4. The output end of the motor is connected to a rotating shaft 60. The rotating shaft 60 is located inside the heat transfer oil tank 4. The rotating wheel 59 is connected to the rotating shaft 60. The surface of the rotating shaft 60 is provided with a plurality of blades 61 in the vertical direction.

[0121] The heating components inside the heat transfer oil tank 4 include: a heating plate 57 and a heating block 62;

[0122] The heating block 62 includes a plurality of arc-shaped plates connected in sequence, the diameter of the arc-shaped plates increasing sequentially, and the bottom of the arc-shaped plates being located on the same plane;

[0123] The heating plate 57 is located below the rotating wheel 59. The front and rear sides and the left side of the heating plate 57 are respectively sealed to the front and rear side walls and the left side wall of the heat transfer oil tank 4. A gap is left between the right side of the heating plate 57 and the right side wall of the heat transfer oil tank 4.

[0124] Multiple heating blocks 62 are provided and connected in sequence to form a staircase-like structure. The heating block 62 near the right side of the heat transfer oil tank 4 is higher than the heating block 62 near the left side of the heat transfer oil tank 4.

[0125] The heating block 62 is located below the heating plate. The right side and front and rear sides of the heating block 62 are sealed to the right side and front and rear side walls of the heat transfer oil tank 4, respectively. A gap is left between the left side of the heating block 62 and the left side wall of the heat transfer oil tank 4.

[0126] When the heat transfer oil is injected at high speed into the heat transfer oil tank, it comes into direct contact with the rotating wheel. The wheel's rotation disperses the oil into a mist, which then falls onto the heating plate. The heating plate heats the oil. As more oil is added, it gradually flows towards the right side of the heating plate, creating a gradual upward flow. This extends the contact time between the oil and the heating plate. Several protrusions on the top surface of the heating plate agitate the oil as it moves, ensuring a uniform temperature rise. Then, the heat transfer oil falls from the right side of the heating plate onto the heating block. Since the heating block is shaped like a staircase, the heat transfer oil flows downhill through the layers. This process can both stir the heat transfer oil and achieve the heating effect. When the temperature sensor detects that the oil temperature is within the set range, the heat transfer oil is drawn away by the oil pump 4. If the heat transfer oil temperature does not reach the set value, heating can continue. To prevent the heat transfer oil tank from filling up, the heat transfer oil tank can be directed to the cooling pipe, but the cooling process is not started. The cooling pipe is used as a return pipe at this time.

[0127] In some embodiments, in order to further increase the contact time between the heat transfer oil and the heating plate, a first support plate 63 and a second support plate 64 are provided in the heat transfer oil tank;

[0128] The first support plate 63 and the second support plate 64 are disposed between the heating block and the heating plate. The left side of the first support plate 63 is connected to the left inner wall of the heat transfer oil tank through a first rotating shaft 67. A groove is provided on the inner wall of the heat transfer oil tank, and the rotating shaft is rotatably connected in the groove.

[0129] The left side of the first support plate 63 is connected to the rotating shaft, the top of the first support plate 63 is connected to the heating plate, and the first support plate 63 is provided with a through hole that corresponds to the position of the protrusion on the heating plate, and the lower end of the protrusion passes through the corresponding through hole.

[0130] The second support plate 64 is located below the first support plate 63, and the first support plate 63 and the second support plate 64 are connected by a first connecting plate 65 and a second connecting plate 66.

[0131] An electric telescopic rod 74 is provided on the top of the heat transfer oil tank. The moving part of the electric telescopic rod 74 is located inside the heat transfer oil tank and is rotatably connected to the right side of the first support through a first ring 73. When the computer controls the electric telescopic rod 74 to move, the first support plate 63 tilts.

[0132] A motor 75 is provided on the outer left side of the heat transfer oil tank. A second rotating shaft 69 is provided at the output end of the motor 75. One end of the second rotating shaft 69 is located inside the heat transfer oil tank. A second ring 70 located inside the heat transfer oil tank is provided at the end of the second rotating shaft 69.

[0133] A third rotating shaft 68 is provided between the first connecting plate 65 and the second connecting plate 66. One end of the third rotating shaft 68 passes through the first connecting plate 65 and is rotatably connected to the second ring 70 through the third ring 71. The other end of the third rotating shaft 68 is rotatably connected to the second connecting plate 66.

[0134] The third rotating shaft 68 is provided with a plurality of cams 72 adapted to the position of the protrusion. The cams 72 respectively contact the corresponding protrusion. When the computer-controlled motor 75 is activated, the second rotating shaft 69 and the third rotating shaft 68 rotate, synchronously driving the cams 72 to rotate. At the same time, the protrusion performs a vertical extension and retraction action on the corresponding arc plate.

[0135] The time it takes for the heat transfer oil to flow through the heating plate can be controlled in several ways:

[0136] The first method involves starting the motor via computer control. The motor drives the second and third rotating shafts to rotate, which in turn causes the cam to rotate. The rotation of the cam causes the protrusion to move, protruding from the heating plate and creating a blocking effect on the heat transfer oil. At the same time, it can change the flow direction of the heat transfer oil, thus slowing down the flow rate of the heat transfer oil on the heating plate and also stirring the heat transfer oil, making the heat transfer oil heat up more evenly and faster.

[0137] In the second method, the electric telescopic rod is started by computer control. The actuating component of the electric telescopic rod drives the first support plate and the second support plate to rotate along the first rotating shaft. The first support plate is close to the top of the heat transfer oil tank, which can block the heat transfer oil, so that the heat transfer oil flows through the heating plate more slowly, thereby increasing the contact time between the heat transfer oil and the heating plate, thus making the heat transfer oil heat up more evenly and faster.

[0138] The third method involves computer control. If the electric telescopic rod is activated, the actuator of the electric telescopic rod will drive the first and second support plates to rotate along the first shaft. The first support plate is close to the bottom of the heat transfer oil tank, which can guide the heat transfer oil, allowing the heat transfer oil to flow through the heating plate more quickly, thereby reducing the contact time between the heat transfer oil and the heating plate.

[0139] The first and second methods are used when the temperature range of the heat transfer oil is large, while the third method is used when the temperature range of the heat transfer oil is small. In actual operation, the control can be made according to the real-time detection results of the temperature sensor.

[0140] In some embodiments, the first temperature control component includes: a first temperature transmitter 6, a second temperature transmitter 7, a first heating chamber 8, a first remote control valve 9, a second remote control valve 10, and a third remote control valve 11;

[0141] The output end of the oil pump 12 is provided with a flow divider pipe, and the output end of the flow divider pipe is provided with three branches, namely the first branch, the second branch and the third branch, which are respectively connected to the first temperature control component, the second temperature control component and the third temperature control component;

[0142] The first branch includes: a first oil pipe 13 and a first return assembly;

[0143] One end of the first oil pipe 13 is connected to the diversion pipe, and the other end of the first oil pipe 13 is connected to one end of the spiral tube on the first reactor 1.

[0144] The first temperature transmitter 6 and the first remote control valve 9 are sequentially arranged on the first oil pipe 13, with the first temperature transmitter 6 located close to the shunt pipe.

[0145] The first reflux assembly includes: a first pipe 14, a second pipe 15, and a third pipe 16;

[0146] One end of the first pipe 14 is connected to the first oil pipe 13 between the first temperature transmitter 6 and the first remote control valve 9, and the other end of the first pipe 14 is connected to the input end of the first heating box 8.

[0147] One end of the second pipe 15 is connected to the output end of the first heating box 8, and the other end of the second pipe 15 is connected to the first oil pipe 13 between the first remote control valve 9 and the first reaction vessel 1.

[0148] One end of the third pipe 16 is connected to the second pipe 15, and the other end of the third pipe 16 is connected to the top of the first heating box 8;

[0149] The third remote control valve 11 is installed on the first pipe 14, the second temperature transmitter 7 and the second remote control valve 10 are both installed on the second pipe 15, the second remote control valve 10 is located on the second pipe 15 between the third pipe 16 and the first oil pipe 13, and the second temperature transmitter 7 is located on the second pipe 15 between the second remote control valve 10 and the first heating box 8.

[0150] When the first reactor is operating, a flame retardant is prepared. Under nitrogen protection, a catalyst is added to the first reactor. A temperature sensor monitors the oil temperature in the heat transfer oil tank in real time. If the oil temperature is lower than the set range, a computer-controlled current flows through the heating plate and heating block. The heating plate and heating block generate heat to raise the temperature of the heat transfer oil. The temperature sensor monitors the oil temperature in the heat transfer oil tank in real time until the oil temperature rises to within the set range. Then, the oil pump delivers the heat transfer oil to the first oil pipe. The first temperature transmitter then detects the oil temperature. If the oil temperature is within the set range, the first remote control valve opens, and the second and third remote control valves close, allowing the heat transfer oil to directly enter the spiral tube on the first reactor. If the oil temperature is within the set range... If there is a loss during the process, and the temperature falls below the set range, both the first and second remote control valves will be closed, while the third remote control valve will be opened. The heat transfer oil will enter the first heating chamber for heating to compensate for the oil temperature. The oil temperature will then be monitored by the second temperature transmitter until it reaches the set range. The second remote control valve will then be opened, allowing the heat transfer oil to enter the spiral tube on the first reactor. The stirrer will be controlled to stir the added material, and the solenoid valve on the trimethyl phosphite storage tank will be opened to add trimethyl phosphite dropwise into the first reactor. After the addition is complete, the mixture will be heated to reflux and reacted at atmospheric pressure for 5–6 hours. The fraction collected at 97–1-5℃ / 5KPa will be distilled under reduced pressure, which is dimethyl methylphosphonate.

[0151] In some embodiments, the second temperature control component includes: a third temperature transmitter 17, a fourth temperature transmitter 18, a second heating chamber 19, a fourth remote control valve 20, a fifth remote control valve 21, and a sixth remote control valve 22.

[0152] The second branch includes: a second oil pipe 23 and a second return assembly;

[0153] One end of the second oil pipe 23 is connected to the diversion pipe, and the other end of the second oil pipe 23 is connected to one end of the spiral tube on the second reactor 2;

[0154] The third temperature transmitter 17 and the fourth remote control valve 20 are sequentially arranged on the second oil pipe 23, with the third temperature transmitter 17 located close to the shunt pipe.

[0155] The second return pipe includes: a fourth pipe 24, a fifth pipe 25, and a sixth pipe 58;

[0156] One end of the fourth pipe 24 is connected to the second oil pipe 23 between the third temperature transmitter 17 and the fourth remote control valve 20, and the other end of the fourth pipe 24 is connected to the input end of the second heating box 19.

[0157] One end of the fifth pipe 25 is connected to the output end of the second heating box 19, and the other end of the fifth pipe 25 is connected to the second oil pipe 23 between the fourth remote control valve 20 and the second reaction vessel 2.

[0158] One end of the sixth pipe 58 is connected to the fifth pipe 25, and the other end of the sixth pipe 58 is connected to the top of the second heating box 19;

[0159] The sixth remote control valve 22 is installed on the fourth pipe 24, the fourth temperature transmitter 18 and the fifth remote control valve 21 are both installed on the fifth pipe 25, the fifth remote control valve 21 is located on the fifth pipe 25 between the sixth pipe 58 and the second oil pipe 23, and the fourth temperature transmitter 18 is located on the fifth pipe 25 between the fifth remote control valve 21 and the second heating box 19.

[0160] When the second reactor is operating, i.e., preparing unsaturated polyester resin, isophthalic acid, fumaric acid, pentaerythritol, D-33 diol, and a modifier / modified molecular sieve catalyst are added to the second reactor under nitrogen protection. Nitrogen is continuously introduced after the addition is complete. A temperature sensor continuously monitors the oil temperature in the heat transfer oil tank. If the oil temperature is lower than the set range, a computer-controlled current flows through the heating plate and heating block, which heat the heat transfer oil. The temperature sensor continuously monitors the oil temperature in the heat transfer oil tank until the oil temperature rises to within the set range. Then, the oil pump delivers the heat transfer oil to the second oil pipe. A third temperature transmitter then monitors the oil temperature. If the oil temperature is within the set range, it directly enters the spiral tube on the second reactor. If the oil temperature is lost during transportation and falls below the set range, the fourth and fifth remote control valves will be closed, and the sixth remote control valve will be opened. The heat transfer oil will enter the second heating box for heating to compensate for the oil temperature. The oil temperature will then be monitored by the fourth temperature transmitter until it reaches the set range. The fifth remote control valve will then be opened, and the heat transfer oil will enter the spiral tube on the second reactor. The stirrer on the second reactor will then be controlled to stir the added material. The heating temperature is 165-185℃, the heating rate is 12-15℃ / h, and the reaction continues for 25-35 minutes. Then the temperature will be further increased to 245-260℃, the heating rate is 2-3℃ / h, and the stirring continues for 2.5-3 hours to obtain the unsaturated polyester resin solution.

[0161] In some embodiments, the third temperature control component includes: a fifth temperature transmitter 26, a sixth temperature transmitter 27, a third heating chamber 28, a seventh remote control valve 29, an eighth remote control valve 30, and a ninth remote control valve 31;

[0162] The third branch includes: a third oil pipe 32 and a third return assembly;

[0163] One end of the third oil pipe 32 is connected to the diversion pipe, and the other end of the third oil pipe 32 is connected to one end of the spiral tube on the third reactor 3;

[0164] The fifth temperature transmitter 26 and the seventh remote control valve 29 are sequentially arranged on the third oil pipe 32, and the fifth temperature transmitter 26 is arranged close to the shunt pipe;

[0165] The third reflux assembly includes: a seventh pipe 33, an eighth pipe 34, and a ninth pipe 35;

[0166] One end of the seventh pipe 33 is connected to the third oil pipe 32 between the fifth temperature transmitter 26 and the seventh remote control valve 29, and the other end of the seventh pipe 33 is connected to the input end of the third heating box 28.

[0167] One end of the eighth pipe 34 is connected to the output end of the third heating box 28, and the other end of the eighth pipe 34 is connected to the third oil pipe 32 between the seventh remote control valve 29 and the third reaction vessel 3;

[0168] One end of the ninth pipe 35 is connected to the eighth pipe 34, and the other end of the ninth pipe 35 is connected to the top of the third heating box 28.

[0169] The ninth remote control valve 31 is installed on the seventh pipe 33, the sixth temperature transmitter 27 and the eighth remote control valve 30 are both installed on the eighth pipe 34, the eighth remote control valve 30 is located on the eighth pipe 34 between the ninth pipe 35 and the third oil pipe 32, and the sixth temperature transmitter 27 is located on the eighth pipe 34 between the eighth remote control valve 30 and the third heating box 28.

[0170] The above three heating boxes are all existing structures, and their working principles will not be described in detail. For example, the heating box can be equipped with an electric heating wire or heating plate inside the box, and the electric heating wire or heating plate can be connected to an external power source.

[0171] In the process of synthesizing flame-retardant unsaturated resin in the third reactor, the prepared dimethyl methylphosphonate, anhydrous ethanol, aluminum trioxide, and sodium hydroxide solution are added to the third reactor. The stirring mechanism on the third reactor is controlled to stir and dissolve the added materials, and then the prepared unsaturated polyester resin is added. A temperature sensor monitors the oil temperature in the heat transfer oil tank in real time. If the oil temperature is lower than the set range, the computer controls the current to pass through the heating plate and heating block. The heating plate and heating block generate heat to raise the temperature of the heat transfer oil. The temperature sensor monitors the oil temperature in the heat transfer oil tank in real time until the oil temperature rises to within the set range. Then, the oil pump delivers the heat transfer oil to the third oil pipe. The fifth temperature transmitter then monitors the oil temperature. If the oil temperature is within the set range, it directly enters the spiral tube on the third reactor. If the oil temperature drops below the set range during transportation, the seventh and eighth remote control valves are closed, and the ninth remote control valve is opened. The heat transfer oil enters the third heating box for heating to compensate for the oil temperature. The oil temperature is then monitored by the sixth temperature transmitter until it returns to the set range. The eighth remote control valve is then opened, and the heat transfer oil enters the spiral tube on the third reactor. The stirrer on the third reactor is then controlled to stir the mixture for 3.5–4.5 hours. The temperature is then raised to 85–90°C, and a saturated potassium carbonate solution is added. After stirring for another 3.5–4.5 hours, diaminosilane is added dropwise, and diethylene glycol acetate is continuously added to maintain a certain fluidity of the material. After rotary evaporation of the solvent, the product is washed until neutral and dried to obtain a flame-retardant unsaturated polyester resin.

[0172] In some embodiments, the input end of the heat transfer oil tank 4 is provided with an oil return pipe;

[0173] The other ends of the spiral tubes on the first reactor 1, the second reactor 2, and the third reactor 3 are respectively connected to the return oil pipe through the first circuit pipe 36, the second circuit pipe 37, and the third circuit pipe 38; the first circuit pipe 36, the second circuit pipe 37, and the third circuit pipe 38 are respectively provided with a tenth remote control valve 39, an eleventh remote control valve 40, and a twelfth remote control valve 41; the return oil pipe is provided with an eighth temperature transmitter 42 and a thirteenth remote control valve 43; the thirteenth remote control valve 43 is located near the input end of the heat transfer oil tank 4.

[0174] Specifically, when the first reactor is working, the tenth remote control valve is open, the eleventh and twelfth remote control valves are closed, and the thirteenth remote control valve is open. When the second reactor is working, the tenth remote control valve is closed, the eleventh remote control valve is open, the twelfth remote control valve is closed, and the thirteenth remote control valve is open. When the third reactor is working, the tenth and eleventh remote control valves are closed, the twelfth remote control valve is open, and the thirteenth remote control valve is open. The function of the eighth temperature transmitter is to detect the temperature of the heat transfer oil when it enters the heat transfer oil tank, and thus control the current flowing into the heating plate and heating block according to the detected temperature.

[0175] Example 2

[0176] A method for preparing a flame-retardant unsaturated polyester resin, wherein the preparation method is applied in the above-mentioned preparation system and includes:

[0177] To prepare the flame retardant, a catalyst is added to the first reactor 1 under nitrogen protection. A temperature sensor monitors the oil temperature in real time. If the oil temperature is below a set range, the computer controls the heating components to heat the heat transfer oil. The temperature sensor monitors the oil temperature in the heat transfer oil tank 4 in real time until the oil temperature rises to the set range of 0-5°C. Then, the oil pump 12 delivers the heat transfer oil to the first oil pipe 13. The first temperature transmitter 6 monitors the oil temperature. If the oil temperature is within the set range, it directly enters the spiral tube on the first reactor 1. If the oil temperature is lost during delivery and falls below the set range, the heat transfer oil is controlled to enter the first heating box 8. Heating is performed to compensate for the oil temperature, and then the oil temperature is detected by the second temperature transmitter 7 until the oil temperature reaches the set range. Then, the heat transfer oil is controlled to enter the spiral tube on the first reactor 1. Then, the stirrer is controlled to stir the added material, and the solenoid valve on the trimethyl phosphite storage tank is controlled to open, so that trimethyl phosphite is added dropwise to the first reactor 1. After the dropwise addition is completed, the mixture is heated to reflux and reacted at atmospheric pressure for 5 to 6 hours. The fraction with a temperature of 97 to 1-5℃ / 5KPa is collected by vacuum distillation, which is dimethyl methylphosphonate. The catalyst used is methyl p-toluenesulfonate, and the mass ratio of the catalyst to trimethyl phosphite is 1:9.

[0178] Under nitrogen protection, isophthalic acid, fumaric acid, pentaerythritol, D-33 diol, and a modified molecular sieve catalyst were first added to the reactor. After the addition was complete, nitrogen gas was continuously introduced, and the mixture was stirred and heated to 165–185°C at a heating rate of 12–15°C / h. The reaction was continued for 25–35 min, and then the temperature was further increased to 245–260°C at a heating rate of 2–3°C / h. After stirring for 2.5–3 h, an unsaturated polyester resin solution was obtained. The modified agent was a mixture of cyclopentene and 1,4-cyclohexadiene in a molar ratio of 1:1.2. The alumina particle size was 30 nm.

[0179] To prepare unsaturated polyester resin, under nitrogen protection, isophthalic acid, fumaric acid, pentaerythritol, D-33 diol, and a modified molecular sieve catalyst are first added to the second reactor. After addition, nitrogen is continuously purged. A temperature sensor monitors the oil temperature in real time. If the oil temperature is lower than a set range, the computer controls the heating element to heat the heat transfer oil. The temperature in the heat transfer oil tank 4 is monitored in real time by the temperature sensor until the oil temperature rises to 165-185℃, with a heating rate of 12-15℃ / h. Then, oil pump 12 delivers the heat transfer oil to the second oil pipe 23, and the third temperature transmitter 17 monitors the oil temperature. If the oil temperature is within the set range... Within the set range, the oil directly enters the spiral tube on the second reactor 2. If the oil temperature is lost during the transportation process and falls below the set range, the heat transfer oil is controlled to enter the second heating box 19 for heating to compensate for the oil temperature. Then, the oil temperature is detected by the fourth temperature transmitter until the oil temperature returns to the set range. Then, the heat transfer oil is controlled to enter the spiral tube on the second reactor 2, and the stirrer on the second reactor 2 is controlled to stir the added material. The reaction continues for 25-35 minutes, and then the temperature is raised to 245-260℃ at a rate of 2-3℃ / h. After stirring for 2.5-3 hours, the unsaturated polyester resin solution is obtained.

[0180] Synthesis of flame-retardant unsaturated resin: Dimethyl methylphosphonate, anhydrous ethanol, aluminum oxide, and sodium hydroxide solution are added to the third reactor 3, along with the prepared unsaturated polyester resin. The stirring mechanism on the third reactor is controlled to stir the materials until they dissolve. A temperature sensor continuously monitors the oil temperature in the heat transfer oil tank. If the oil temperature is below the set range, a computer-controlled current flows through the heating plate and heating block, raising the temperature of the heat transfer oil. The temperature sensor continuously monitors the oil temperature in the heat transfer oil tank until it rises to the set range. Then, the oil pump delivers the heat transfer oil to the third oil pipe. The fifth temperature transmitter then monitors the oil temperature. If the oil temperature is within the set range, the seventh remote control valve opens, and the eighth and ninth remote control valves close, allowing the heat transfer oil to directly enter the third reactor. If the oil temperature drops below the set range during transport in the spiral tube, both the seventh and eighth remote control valves are closed, and the ninth remote control valve is opened. The heat transfer oil enters the third heating box for heating to compensate for the oil temperature. The oil temperature is then monitored by the sixth temperature transmitter until it reaches 40-45°C. Then, the eighth remote control valve is opened, and the heat transfer oil enters the spiral tube on the third reactor. The stirrer is then used to stir the added material for 3.5-4.5 hours. The temperature is then raised to 85-90°C, and a saturated potassium carbonate solution is added. After stirring for 3.5-4.5 hours, diaminosilane is added dropwise, and diethylene glycol acetate is continuously added to maintain a certain fluidity of the material. After rotary evaporation of the solvent, the product is washed until neutral and dried to obtain a flame-retardant unsaturated polyester resin.

[0181] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A flame retardant unsaturated polyester resin preparation system characterized by comprising: The application relates to a temperature control system for a first reactor, a second reactor and a third reactor. The temperature control system comprises a heating system and a cooling system. The heating system comprises a heat conduction oil tank and a temperature control assembly connected with the heat conduction oil tank. The heat conduction oil tank is provided with a temperature sensor and a heating assembly for heating the heat conduction oil. The temperature control assembly comprises a first temperature control assembly, a second temperature control assembly and a third temperature control assembly connected with the first reactor, the second reactor and the third reactor respectively. The first temperature control assembly, the second temperature control assembly and the third temperature control assembly are also connected with the cooling system and the heat conduction oil tank respectively. The heat conduction oil tank is provided with a first output end and a second output end. The first output end is connected with an oil pump. The oil pump is connected with the first temperature control assembly, the second temperature control assembly and the third temperature control assembly respectively. The heat conduction oil tank is provided with an oil diffusion assembly for diffusing the heat conduction oil in the heat conduction oil tank. The oil diffusion assembly comprises a motor and a rotating wheel. The motor is connected with the outer surface of the heat conduction oil tank. The output end of the motor is connected with a rotating shaft. The rotating shaft is located in the heat conduction oil tank. The rotating wheel is connected with the rotating shaft. The rotating shaft is provided with a plurality of blades in the vertical direction. The heating assembly in the heat conduction oil tank comprises a heating plate and a heating block. The heating block comprises a plurality of arc-shaped plates connected in sequence. The diameters of the arc-shaped plates increase in sequence. The bottoms of the arc-shaped plates are located on the same plane. The heating plate is located below the rotating wheel. The front and back sides and the left side of the heating plate are tightly attached with the front and back walls and the left wall of the heat conduction oil tank respectively. The right side of the heating plate is spaced apart from the right wall of the heat conduction oil tank. The heating block is provided with a plurality of heating blocks connected in sequence in a stair-like structure. The heating block close to the right side of the heat conduction oil tank is higher than the heating block close to the left side of the heat conduction oil tank. The heating block is located below the heating plate. The right side and the front and back sides of the heating block are tightly attached with the right side and the front and back walls of the heat conduction oil tank respectively. The left side of the heating block is spaced apart from the left wall of the heat conduction oil tank. When the heat conduction oil is sprayed into the heat conduction oil tank at high speed, the heat conduction oil is in contact with the front surface of the rotating wheel. The rotating wheel diffuses the heat conduction oil into oil mist and then drops on the heating plate. The heating plate heats the heat conduction oil. With the increase of the heat conduction oil, the heat conduction oil flows to the right side of the heating plate and then drops on the heating block from the right side of the heating plate. Finally, the heat conduction oil flows to the bottom of the heat conduction oil tank and is pumped away by the oil pump. The first temperature control assembly, the second temperature control assembly and the third temperature control assembly are used for compensating the temperature of the heat conducting oil when the first reactor, the second reactor and the third reactor work, so that the temperature of the heat conducting oil is controlled in a required range; the cooling system is used for cooling the heat conducting oil in the heat conducting oil tank and then supplying the first reactor, the second reactor and the third reactor respectively; in the temperature control process, the actions of various elements are controlled by an external computer.

2. The fire-retardant unsaturated polyester resin preparation system according to claim 1, characterized by, The first reactor, the second reactor and the third reactor are all provided with heat preservation shells in the outer sides, and the heat preservation shells are in a closed cavity structure; Spiral pipes are arranged in the heat preservation shells, one end of the spiral pipes penetrates through the heat preservation shells and is connected with the output ends of the first temperature control assembly, the second temperature control assembly and the third temperature control assembly respectively, and the other end of the spiral pipes penetrates through the heat preservation shells and is connected with the heat conducting oil tank.

3. The fire-retardant unsaturated polyester resin preparation system according to claim 1, characterized by, The first temperature control assembly comprises a first temperature transmitter, a second temperature transmitter, a first heating tank, a first remote control valve, a second remote control valve and a third remote control valve; The output end of the oil pump is provided with a shunt pipe, the output end of the shunt pipe is provided with three branches, which are a first branch, a second branch and a third branch respectively, and the first branch, the second branch and the third branch are connected with the first temperature control assembly, the second temperature control assembly and the third temperature control assembly respectively; The first branch comprises a first oil pipe and a first return assembly; One end of the first oil pipe is connected with the shunt pipe, and the other end of the first oil pipe is connected with one end of the spiral pipe on the first reactor; The first temperature transmitter and the first remote control valve are sequentially arranged on the first oil pipe, and the first temperature transmitter is arranged close to the shunt pipe; The first return assembly comprises a first pipeline, a second pipeline and a third pipeline; One end of the first pipeline is connected with the first oil pipe between the first temperature transmitter and the first remote control valve, and the other end of the first pipeline is connected with the input end of the first heating tank; One end of the second pipeline is connected with the output end of the first heating tank, and the other end of the second pipeline is connected with the first oil pipe between the first remote control valve and the first reactor; One end of the third pipeline is connected with the second pipeline, and the other end of the third pipeline is connected with the top of the first heating tank; The third remote control valve is installed on the first pipeline, the second temperature transmitter and the second remote control valve are both installed on the second pipeline, the second remote control valve is located on the second pipeline between the third pipeline and the first oil pipe, and the second temperature transmitter is located on the second pipeline between the second remote control valve and the first heating tank.

4. The fire-retardant unsaturated polyester resin preparation system according to claim 3, characterized by, The second temperature control assembly comprises a third temperature transmitter, a fourth temperature transmitter, a second heating tank, a fourth remote control valve, a fifth remote control valve and a sixth remote control valve; The second branch comprises a second oil pipe and a second return assembly; One end of the second oil pipe is connected with the shunt pipe, and the other end of the second oil pipe is connected with one end of the spiral pipe on the second reactor; The third temperature transmitter is arranged on the second oil pipe, and the fourth remote control valve is arranged on the third oil pipe; The second return assembly comprises a fourth pipe, a fifth pipe and a sixth pipe; One end of the fourth pipe is connected with the second oil pipe between the third temperature transmitter and the fourth remote control valve, and the other end of the fourth pipe is connected with the input end of the second heating tank; One end of the fifth pipe is connected with the output end of the second heating tank, and the other end of the fifth pipe is connected with the second oil pipe between the fourth remote control valve and the second reaction kettle; One end of the sixth pipe is connected with the fifth pipe, and the other end of the sixth pipe is connected with the top of the second heating tank; The fourth temperature transmitter and the fifth remote control valve are arranged on the fifth pipe, and the fifth remote control valve is arranged on the fifth pipe between the sixth pipe and the second oil pipe, and the fourth temperature transmitter is arranged on the fifth pipe between the fifth remote control valve and the second heating tank.

5. The fire-retardant unsaturated polyester resin preparation system according to claim 3, wherein The third temperature control assembly comprises a fifth temperature transmitter, a sixth temperature transmitter, a third heating tank, a seventh remote control valve, an eighth remote control valve and a ninth remote control valve; The third branch comprises a third oil pipe and a third return assembly; One end of the third oil pipe is connected with the shunt pipe, and the other end of the third oil pipe is connected with one end of the spiral pipe on the third reaction kettle; The fifth temperature transmitter is arranged on the third oil pipe, and the seventh remote control valve is arranged on the third oil pipe; The third return assembly comprises a seventh pipe, an eighth pipe and a ninth pipe; One end of the seventh pipe is connected with the third oil pipe between the fifth temperature transmitter and the seventh remote control valve, and the other end of the seventh pipe is connected with the input end of the third heating tank; One end of the eighth pipe is connected with the output end of the third heating tank, and the other end of the eighth pipe is connected with the third oil pipe between the seventh remote control valve and the third reaction kettle; One end of the ninth pipe is connected with the eighth pipe, and the other end of the ninth pipe is connected with the top of the third heating tank; The ninth remote control valve is arranged on the seventh pipe, and the sixth temperature transmitter and the eighth remote control valve are arranged on the eighth pipe, and the eighth remote control valve is arranged on the eighth pipe between the ninth pipe and the third oil pipe, and the sixth temperature transmitter is arranged on the eighth pipe between the eighth remote control valve and the third heating tank.

6. The fire-retardant unsaturated polyester resin preparation system according to claim 2, wherein The input end of the heat conducting oil tank is provided with an oil return pipe; The other ends of the spiral pipes on the first reaction kettle, the second reaction kettle and the third reaction kettle are respectively connected with the oil return pipe through a first return pipe, a second return pipe and a third return pipe; the first return pipe, the second return pipe and the third return pipe are respectively provided with a tenth remote control valve, an eleventh remote control valve and a twelfth remote control valve, the oil return pipe is provided with an eighth temperature transmitter and a thirteenth remote control valve, and the thirteenth remote control valve is arranged close to the input end of the heat conducting oil tank.

7. The fire-retardant unsaturated polyester resin preparation system according to claim 1, wherein The cooling system comprises a liquid cooling assembly, a gas cooling assembly and an incubator; The liquid cooling assembly comprises a liquid storage tank, a first delivery pump and a first elbow pipe; The liquid storage tank is filled with cooling liquid, and the input end and the output end of the first delivery pump are connected with the pipelines on both sides of the liquid storage tank respectively; The first elbow pipe is arranged on the pipeline between the output end of the first delivery pump and the liquid storage tank; The gas cooling assembly comprises a refrigerant medium tank, a second delivery pump and a second elbow pipe; The refrigerant medium tank is filled with refrigerant medium, and the input end and the output end of the second delivery pump are connected with the pipelines on both sides of the refrigerant medium tank respectively The second elbow pipe is arranged on the pipeline between the output end of the second delivery pump and the refrigerant medium tank; The second output end of the heat conducting oil tank is connected with a cooling pipe through a pipeline, the cooling pipe is arranged between the first elbow pipe and the second elbow pipe, and the cooling pipe is in close contact with the first elbow pipe and the second elbow pipe; The first elbow pipe, the second elbow pipe and the cooling pipe are arranged in the incubator, the end of the cooling pipe is connected with the pipeline between the heat conducting oil tank and the oil pump through a pipeline, a seventh temperature transmitter is arranged on the pipeline, the seventh temperature transmitter is arranged close to the incubator, a branch pipeline is arranged between the pipeline and the heat conducting oil tank, and a sixteenth remote control valve is arranged on the branch pipeline; A fourteenth remote control valve is arranged on the pipeline between the heat conducting oil tank and the oil pump, a fifteenth remote control valve is arranged on the pipeline between the cooling pipe and the heat conducting oil tank, and a seventeenth remote control valve is arranged on the pipeline between the cooling pipe and the oil pump.

8. The fire-retardant unsaturated polyester resin preparation system according to claim 1, wherein First and second support plates are arranged in the heat conducting oil tank; The first and second support plates are arranged between the heating block and the heating plate, the left side of the first support plate is connected with the left inner wall of the heat conducting oil tank through a first rotating shaft, a groove is arranged on the inner wall of the heat conducting oil tank, and the rotating shaft is rotatably connected in the groove; The left side of the first support plate is connected with the rotating shaft, the top of the first support plate is connected with the heating plate, a through hole is arranged on the first support plate and corresponding to the protruding position on the heating plate, and the lower end of the protrusion passes through the corresponding through hole; The second support plate is arranged below the first support plate, and the first and second support plates are connected through first and second connecting plates; An electric telescopic rod is arranged on the top of the heat conducting oil tank, the moving part of the electric telescopic rod is arranged in the heat conducting oil tank and rotatably connected with the right side of the first support plate, and when the electric telescopic rod is actuated by the computer, the first support plate is inclined; An electric motor is arranged on the left outer surface of the heat conducting oil tank, a second rotating shaft is arranged at the output end of the electric motor, one end of the second rotating shaft is arranged in the heat conducting oil tank, and a second ring is arranged on the end of the second rotating shaft and arranged in the heat conducting oil tank. A third rotating shaft is arranged between the first connecting plate and the second connecting plate, one end of the third rotating shaft is connected with the second ring through a third ring, and the other end of the third rotating shaft is rotatably connected with the second connecting plate; A plurality of cams corresponding to the convex positions are arranged on the third rotating shaft, the cams are respectively in contact with the corresponding convexes, when the computer-controlled motor is actuated, the second rotating shaft and the third rotating shaft rotate, and the cams are driven to rotate at the same time, and the convexes are vertically expanded and contracted on the corresponding arc-shaped plates.

9. 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computer is controlled to heat to 40-45 DEG C, then the stirrer on the third reaction kettle is controlled to stir, the reaction is carried out for 3.5-4.5 h, then the temperature is raised to 85-90 DEG C, saturated potassium carbonate solution is added, the stirring reaction is carried out for 3.5-4.5 h, then diaminosilane is added dropwise, and diethylene glycol acetate is continuously added to keep the material in a certain fluidity, the solvent is removed by rotary evaporation, the product is washed to neutral, and dried to obtain the flame-retardant unsaturated polyester resin.

Citation Information

Patent Citations

  • Preparation method of flame retardant unsaturated polyester resin

    CN115028822B

  • Natural gas flow measuring system self-adaptive to ambient temperature

    CN110595558A

  • Preparation method of flame-retardant unsaturated polyester resin

    CN115028822A

  • Synthesis device of isocyanate prepolymer

    CN209302729U

  • Rapid cooling device for plastic stabilizer

    CN210417240U