MQ resin continuous production system

Abstract

The utility model relates to an MQ resin continuous production system which comprises a first storage tank used for containing M and Q chain link sources, a second storage tank used for containing acid liquor, a third storage tank, a flow tube reactor, a constant-temperature reaction tank, a neutralization kettle and a drying module, and the output end of the first storage tank is connected with the input end of the flow tube reactor so that the M and Q chain link sources can be movably conveyed; the output end of the first storage tank is connected with the input end of the first storage tank, the output end of the second storage tank is connected with the input end of the flow tube reactor, the output end of the flow tube reactor is connected with the input end of the neutralization kettle, the output end of the third storage tank is connected with the input end of the neutralization kettle, and the output end of the neutralization kettle is connected with the input end of the drying module. The flow tube reactor is placed in the constant-temperature reaction tank, and the flow tube reactor is arranged in an annular spiral manner. The method has the advantages that the control accuracy of reaction conditions such as temperature in the reaction process is improved, and the situation that a large amount of gel is blocked due to unstable reaction conditions is reduced.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of silicone resins, in particular to a continuous production system of MQ resin. BACKGROUND

[0002] MQ silicone resin is a branched organopolysiloxane composed of monofunctional organosiloxane segments (M) and tetrafunctional siloxane segments (Q) in different proportions.

[0003] MQ resin is usually prepared by sol-gel method in industry, in which the main raw material of M segment is hexamethyldisiloxane or trimethylchlorosilane, and the main raw material of Q segment is sodium silicate (water glass) or tetraethyl orthosilicate; the former is called sodium silicate method (water glass method), and the latter is called tetraethyl orthosilicate method (silicate method). The sodium silicate method is usually used in industrial preparation, and the hydrolysis and polycondensation of M and Q segments are carried out in a reaction kettle, followed by intermittent production of neutralization and drying treatment. However, this method is affected by the molecular weight distribution of the silica sol formed by sodium silicate and the reaction conditions, and the ratio of M and Q segments of MQ silicone resin is difficult to adjust.

[0004] The reaction conditions of the traditional production method are difficult to accurately control, the temperature in the reaction kettle is not accurately and stably controlled, a large amount of gel is easily formed during the reaction process, and the production of large quantities and high-quality MQ organosilicon resin is difficult to meet the production demand. CONTENT OF THE INVENTION

[0005] In order to improve the control accuracy of reaction conditions such as temperature in the reaction process, and reduce the gel blockage caused by unstable reaction conditions, the application provides a continuous production system of MQ resin.

[0006] The application provides a continuous production system of MQ resin, which adopts the following technical scheme:

[0007] The application discloses a continuous production system of MQ resin, which comprises a first storage tank for placing M and Q chain segment sources, a second storage tank for placing acid liquid, a third storage tank for placing alkali liquid, a flow pipe reactor, a constant temperature reaction tank, a neutralization kettle and a drying module, wherein the output end of the first storage tank is connected with the input end of the flow pipe reactor to convey the M and Q chain segment sources into the flow pipe reactor, the output end of the second storage tank is connected with the input end of the flow pipe reactor to convey the acid liquid into the flow pipe reactor, the output end of the flow pipe reactor is connected with the input end of the neutralization kettle to convey the mixed liquid of the M and Q chain segment sources and the acid liquid into the neutralization kettle, the output end of the third storage tank is connected with the input end of the neutralization kettle to convey the alkali liquid into the neutralization kettle, the output end of the neutralization kettle is connected with the input end of the drying module to collect the reacted mixed liquid, and the flow pipe reactor is arranged in the constant temperature reaction tank and is arranged in a ring shape.

[0008] By adopting the above technical scheme, when the M and Q chain segment sources in the first storage tank and the acid liquid in the second storage tank are mixed and then enter the flow pipe reactor to react, the liquid in the constant temperature reaction tank can heat and control the temperature of the immersed flow pipe reactor, the reaction condition can be accurately controlled, the gel generated in the production process of the MQ resin is further reduced, the blockage caused by the gel is reduced, and therefore the reaction accuracy and efficiency of the mixed liquid are improved, so that the production requirement of large-batch and high-quality MQ type silicone resin is met.

[0009] Optionally, a PH value detection device is arranged on the inner side wall of the neutralization kettle.

[0010] By adopting the above technical scheme, after the alkali liquid in the third storage tank enters the neutralization kettle to react with the mixed liquid, the PH value detection device can detect the acid-base degree of the mixed liquid in the neutralization kettle, so that the standard value of the mixed MQ resin liquid after mixing can be judged.

[0011] Optionally, the application further comprises a separator and a liquid storage tank, the input end of the separator is connected with the output end of the neutralization kettle to separate the reacted liquid, the output end of the separator is connected with the input end of the drying module to dry the liquid, and the input end of the liquid storage tank is connected with the output end of the separator to collect the separated waste liquid.

[0012] By adopting the above technical scheme, when the mixed liquid in the neutralization kettle enters the finishing stage, the separator can separate the reacted mixed liquid, the separated MQ type silicone liquid can enter the drying module for subsequent treatment, and the separated water phase waste liquid can enter the liquid storage tank for recycling, so that the production efficiency and speed of the MQ type silicone resin are improved.

[0013] Optionally, the number of the flow tube reactor and the constant temperature reaction tank is at least two and arranged in parallel.

[0014] By adopting the above technical scheme, the number of the flow tube reactor and the constant temperature reaction tank is two, which is more suitable for improving the control accuracy of the temperature and other conditions of the liquid in the overall flow tube reactor, facilitating the control of the staff, reducing the dispersion of the staff's energy, and further improving the reaction efficiency of the liquid.

[0015] Optionally, it further comprises a plurality of metering pumps, and the plurality of metering pumps are respectively and one by one arranged at the input end of the flow tube reactor and the input end of the neutralization kettle to control the flow of the liquid.

[0016] By adopting the above technical scheme, the metering pump arranged between the first storage tank and the flow tube reactor can control the speed and metering of the M and Q chain link source flowing to the flow tube reactor; the metering pump arranged between the second storage tank and the flow tube reactor can control the speed and metering of the acid liquid entering the flow tube reactor; and the metering pump arranged between the third storage tank and the neutralization kettle can control the speed and metering of the alkali entering the neutralization kettle.

[0017] Optionally, the drying module comprises a vacuum distillation tower arranged in the drying module to reduce the generation of impurities in the MQ resin mixed liquid.

[0018] By adopting the above technical scheme, the arrangement of the vacuum distillation tower can perform a preliminary drying treatment on the MQ resin mixed liquid entering the drying module, thereby reducing the generation of impurities in the MQ resin mixed liquid in a short time and facilitating further drying treatment.

[0019] Optionally, a fixed ball is fixedly connected to the inner side wall of the constant temperature reaction tank, and a fixed strip with a deformation force is rotatably connected to the inner side wall of the constant temperature reaction tank, and a through hole in which the fixed ball is sleeved is formed in one end of the fixed strip away from the rotation position.

[0020] By adopting the above technical scheme, the arrangement of the fixed strip and the fixed ball can preliminarily fix the flow tube reactor placed in the constant temperature reaction tank, avoid the flow tube reactor from falling off due to vibration of the equipment during the reaction process, and improve the installation stability of the flow tube reactor.

[0021] Optionally, a slide rail is fixedly connected to the inner side wall of the constant temperature reaction tank, a sliding bead is fixedly connected to one side of the fixed strip away from the through hole, the sliding bead is embedded and slides in the slide rail, an avoidance groove in which part of the fixed strip is clamped is formed in one side of the slide rail close to the fixed ball, the avoidance groove and the slide of the slide rail are in communication with each other, and the number of the avoidance grooves is at least three and arranged in parallel with each other.

[0022] By adopting the above technical scheme, the setting of the slide rail enables the fixing strip to move in at least three gears along the slide rail, so that the actual fastening force of the fixing strip on the flow pipe reactor can be adjusted according to actual conditions, and the position of the flow pipe reactor in the constant-temperature reaction tank can be adjusted.

[0023] To sum up, the present application has at least one of the following beneficial technical effects:

[0024] 1. When the M and Q chain sources in the first storage tank and the acid solution in the second storage tank are mixed and then enter the flow pipe reactor for reaction, the constant-temperature reaction tank controls the temperature of the flow pipe reactor, and the flow pipe reactor is continuously operated in a steady state, so that the mixed solution is uniformly mixed and efficiently reacted under micro-reaction conditions, and uniform flow reaction is not prone to blockage due to gelation, the flow pipe reactor has a large area for heat exchange to ensure the stability of the temperature and increase the reaction sufficiency and efficiency of the mixed solution, so as to meet the production requirements of large quantities and high-quality MQ type silicone resins;

[0025] 2. The setting of the vacuum distillation tower can perform a preliminary drying treatment on the MQ type resin mixed solution entering the drying module, thereby reducing the generation of impurities in the MQ type resin mixed solution in a short time and facilitating further drying treatment.

[0026] 3. The setting of the slide rail enables the fixing strip to move in at least three gears along the slide rail, so that the actual fastening force of the fixing strip on the flow pipe reactor can be adjusted according to actual conditions, and the position of the flow pipe reactor in the constant-temperature reaction tank can be adjusted. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1 is a production flowchart of an MQ resin in the embodiment of the present application.

[0028] Figure 2 is an internal structure diagram of a constant-temperature reaction tank in the embodiment of the present application.

[0029] Marked as follows: 1, first storage tank; 2, second storage tank; 3, third storage tank; 4, flow pipe reactor; 5, constant-temperature reaction tank; 51, fixing assembly; 511, fixing strip; 5112, sliding bead; 5113, through hole; 512, slide rail; 5121, avoiding groove; 513, fixing ball; 6, neutralization kettle; 61, PH value detection device; 7, liquid separator; 8, drying module; 81, liquid storage tank; 82, vacuum distillation tower; 9, metering pump. DETAILED DESCRIPTION

[0030] The following will be described in detail in combination with the accompanying Figures 1-2 The present application will be further described in detail.

[0031] The embodiment of the present application discloses a continuous production system of MQ resin.

[0032] Referring to Figure 1 , a continuous production system of MQ resin comprises a first storage tank 1 for placing M, Q chain source, a second storage tank 2 for placing acid liquid, a third storage tank 3 for placing alkali liquid, a flow tube reactor 4, a constant temperature reaction tank 5, a neutralization kettle 6, a liquid separator 7, a drying module 8 and a liquid storage tank 81. In the embodiment of the application, the above devices are connected by pipelines.

[0033] Referring to Figure 1 , the output end of the first storage tank 1 and the input end of the flow tube reactor 4 are connected by a pipeline, so as to transport the M, Q chain source into the flow tube reactor 4 for reaction. The M, Q chain source is a mixed solution of tetraethyl orthosilicate: hexamethyl siloxane with a weight ratio of 50:15. The output end of the second storage tank 2 and the input end of the flow tube reactor 4 are connected by a pipeline, so as to transport the acid liquid into the flow tube reactor 4 for reaction with the M, Q chain source. The acid liquid in the second storage tank 2 is a mixed liquid of acetic acid: sulfuric acid with a weight ratio of 100:3.

[0034] Referring to Figure 1 , the flow tube reactor 4 is placed in the constant temperature reaction tank 5, so as to facilitate the control of the temperature in the reaction process of the flow tube reactor 4. The number of the flow tube reactor 4 and the constant temperature reaction tank 5 is both two and they are arranged in parallel. The inner diameter of the reaction tube in the flow tube reactor 4 close to the first storage tank 1 and the second storage tank 2 is 5 mm, the volume is 4.5 L, it is made of stainless steel, and the reaction tube is coiled into a ring shape and placed in one of the constant temperature reaction tanks 5. At this time, the temperature in the constant temperature reaction tank 5 is 0-30 degrees Celsius, and the residence time of the mixed liquid in the reaction tube is 0.5 hours. The inner diameter of the reaction tube in the flow tube reactor 4 far away from the first storage tank 1 and the second storage tank 2 is 20 mm, the volume is 25 L, it is also made of stainless steel, and the reaction tube is also coiled into a ring shape and placed in the other constant temperature reaction tank 5. At this time, the temperature in the constant temperature reaction tank 5 is 50-80 degrees Celsius, and the residence time of the mixed liquid in the reaction tube is 3 hours.

[0035] Referring to Figure 1 , the output end of the flow tube reactor 4 far away from the first storage tank 1 and the second storage tank 2 and the input end of the neutralization kettle 6 are connected by a pipeline, so as to transport the mixed liquid of the M, Q chain source and the acid liquid into the neutralization kettle 6 for secondary reaction. The output end of the third storage tank 3 and the input end of the neutralization kettle 6 are connected by a pipeline, so as to transport the alkali liquid in the third storage tank 3 into the neutralization kettle 6 for mixing with the mixed liquid transported out of the flow tube reactor 4. In the embodiment of the application, the neutralization kettle 6 is a conventional reaction kettle which is modified, made of tetrafluoroethylene material and provided with a sandwich temperature control device for cooling by circulating water. The discharge port of the neutralization kettle 6 is provided with a PH value detection device 61 for detecting the acid-base value of the mixed liquid.

[0036] Referring to Figure 1 The pipes are fixedly connected with metering pumps 9, and the number of the metering pumps 9 is four. The first metering pump 9 is installed on the pipe between the first storage tank 1 and the flow tube reactor 4, so as to control the M, Q chain source to enter the flow tube reactor 4 at a flow rate of 0.005 m³ / h. The second metering pump 9 is installed on the pipe between the second storage tank 2 and the flow tube reactor 4, so as to control the acid liquid to enter the flow tube reactor 4 at a flow rate of 0.003 m³ / h. The third metering pump 9 is installed on the pipe between the third storage tank 3 and the neutralization kettle 6, so as to control the alkali liquid (sodium hydroxide) to enter the mixed liquid in the neutralization kettle 6 at a flow rate of 0.04 m³ / h, and the flow rate can be dynamically adjusted according to the PH value. The fourth metering pump 9 is installed on the pipe between the flow tube reactor 4 and the neutralization kettle 6, so as to control the mixed liquid in the flow tube reactor 4 to enter the neutralization kettle 6 at a flow rate of 0.005 m³ / h. The temperature in the neutralization kettle 6 is not higher than 40 degrees Celsius, and the PH value detection device 61 in the neutralization kettle 6 detects the PH value of the mixed liquid to reach 6.5-7.0, so as to control the mixed liquid to be discharged from the neutralization kettle 6.

[0037] Referring to Figure 1 The output end of the neutralization kettle 6 and the input end of the liquid separator 7 are connected through pipes, so as to separate the mixed liquid in the neutralization kettle 6. The output end of the liquid separator 7 is respectively connected with the input end of the drying module 8 and the liquid storage tank 81 through pipes, and the liquid separator 7 separates the mixed liquid into organic phase mixed liquid and water phase waste liquid. The organic phase mixed liquid enters the drying module 8, so as to recover the solvent, and the water phase waste liquid enters the liquid storage tank 81 for recovery. The drying module 8 is fixedly installed with a vacuum distillation tower 82, and the organic phase mixed liquid first enters the vacuum distillation tower 82 in the drying module 8, so as to preliminarily dry the organic phase mixed liquid and reduce impurities. In the embodiment of the application, the liquid separator 7 is a conventional liquid separator in the chemical industry, which is made of tetrafluoroethylene, and the liquid separator 7 automatically discharges the liquid when the liquid in the liquid separator 7 reaches a certain height. The vacuum distillation tower 82 is a conventional vacuum distillation tower 82 in the chemical industry, and the collected organic phase mixed liquid enters the vacuum distillation tower 82. At this time, the vacuum degree is controlled to be-0.05 to-0.1 Mpa, and the temperature is controlled to be 40-60 degrees Celsius, so as to evaporate the organic matter (mainly the reaction byproduct ethyl acetate and small molecule oligomers such as ethanol), and the recovered solid product is subjected to spray drying to obtain the MQ resin product.

[0038] Referring to Figure 1 and Figure 2The inner side wall of the constant-temperature reaction tank 5 is provided with a fixing assembly 51, which comprises a fixing strip 511, a sliding rail 512 and a fixing ball 513. The sliding rail 512 is fixedly connected to the inner side wall of the constant-temperature reaction tank 5 and is arranged along the height of the constant-temperature reaction tank 5. One end of the fixing strip 511 is fixedly connected with a sliding bead 5112, which is embedded in and slides in the sliding groove of the sliding rail 512, so that the fixing strip 511 can move along the length direction of the sliding rail 512. A plurality of fixing balls 513 are fixedly connected to the inner side wall of the constant-temperature reaction tank 5 along the length direction of the track. The end of the fixing strip 511 away from the sliding bead 5112 is provided with a through hole 5113 for the fixing ball 513 to pass through and be clamped, so that the fixing strip 511 can be arranged around and fix the flow pipe reactor 4. The side of the sliding rail 512 close to the fixing strip 511 is provided with an avoiding groove 5121 which is in communication with the inside of the sliding rail 512. When the fixing strip 511 is sleeved on the fixing ball 513, the end of the fixing strip 511 close to the sliding bead 5112 is embedded in the avoiding groove 5121. In the embodiment of the application, the fixing strip 511 has a certain deformation ability, and the number of the fixing strip 511 and the fixing ball 513 is at least three, which are evenly arranged along the length direction of the track, so that the fixing strip 511 can move to control the tightness of the flow channel reactor.

[0039] The implementation principle of the MQ resin continuous production system is that the metering pump 9 controls the M and Q chain source in the first storage tank 1 and the acid liquid in the second storage tank 2 to enter the flow pipe reactor 4 at a certain flow rate for reaction, then the temperature in the first constant-temperature reaction tank 5 is controlled at 0 degrees Celsius, and the temperature in the second constant-temperature reaction tank 5 is 80 degrees Celsius, and the mixed liquid flows at a uniform and slow speed to ensure the residence time of the mixed liquid in the pipe;

[0040] The metering pump 9 controls the mixed liquid in the flow pipe reactor 4 and the alkali liquid in the third storage tank 3 to enter the neutralization kettle 6 at a certain speed for reaction again, the temperature in the neutralization kettle 6 is not higher than 40 degrees Celsius, then the PH value detection device 61 in the neutralization kettle 6 detects the PH value of the mixed liquid to reach 6.5 to control the mixed liquid to be discharged from the neutralization kettle 6, so as to enter the separator 7 for separation, the separated organic phase mixed liquid enters the vacuum distillation tower 82, then the vacuum degree in the vacuum distillation tower 82 is-0.08 Mpa and the temperature is 60 degrees Celsius, so that the organic matter is distilled out, and the recovered solid product is subjected to spray drying in the drying module 8 to obtain the MQ resin product, and the separated aqueous phase waste liquid enters the storage tank 81 for recovery.

[0041] The above are preferred embodiments of the application, which do not limit the protection scope of the application, therefore: any equivalent changes made on the structure, shape and principle of the application should be covered within the protection scope of the application.

Claims

1. A continuous production system of MQ resins, characterized by: The device comprises a first storage tank (1) for placing M, Q chain source, a second storage tank (2) for placing acid, a third storage tank (3) for placing alkali, a flow pipe reactor (4), a constant temperature reaction tank (5), a neutralization kettle (6) and a drying module (8), the output end of the first storage tank (1) is connected with the input end of the flow pipe reactor (4) to deliver M, Q chain source into the flow pipe reactor (4), the output end of the second storage tank (2) is connected with the input end of the flow pipe reactor (4) to deliver acid into the flow pipe reactor (4), the output end of the flow pipe reactor (4) is connected with the input end of the neutralization kettle (6) to deliver the mixture of M, Q chain source and acid into the neutralization kettle (6), the output end of the third storage tank (3) is connected with the input end of the neutralization kettle (6) to deliver alkali into the neutralization kettle (6), the output end of the neutralization kettle (6) is connected with the input end of the drying module (8) to collect the reacted mixture, the flow pipe reactor (4) is placed in the constant temperature reaction tank (5), and the flow pipe reactor (4) is arranged in a ring shape.

2. The system for continuous production of MQ resin according to claim 1, characterized in that: A PH value detection device (61) is arranged on the inner side wall of the neutralization kettle (6).

3. The system for continuous production of MQ resins according to claim 2, characterized in that: The device further comprises a liquid separator (7) and a liquid storage tank (81), the input end of the liquid separator (7) is connected with the output end of the neutralization kettle (6) to separate the reacted liquid, the output end of the liquid separator (7) is connected with the input end of the drying module (8) to dry the liquid, and the input end of the liquid storage tank (81) is connected with the output end of the liquid separator (7) to collect the separated waste liquid.

4. The system for continuous production of MQ resin according to claim 1, characterized in that: The number of the flow pipe reactor (4) and the constant temperature reaction tank (5) is at least two and they are arranged in parallel.

5. The continuous production system of an MQ resin according to claim 2, characterized by: The device further comprises a plurality of metering pumps (9), and each of the metering pumps (9) is arranged at the input end of the flow pipe reactor (4) and the input end of the neutralization kettle (6) to control the flow of liquid.

6. The system for continuous production of MQ resin according to claim 1, characterized in that: The drying module (8) comprises a vacuum distillation tower (82), which is arranged in the drying module (8) to reduce the generation of impurities in the MQ resin mixture.

7. The continuous production system of an MQ resin according to claim 1, characterized by: A fixed ball (513) is fixedly connected to the inner side wall of the constant temperature reaction tank (5), a fixed strip (511) with deformation force is rotatably connected to the inner side wall of the constant temperature reaction tank (5), and a through hole (5113) in which the fixed ball (513) is arranged is formed in one end of the fixed strip (511) away from the rotating position.

8. The system for continuous production of MQ resins according to claim 7, characterized in that: The inner side wall of the constant-temperature reaction tank (5) is fixedly connected with a sliding rail (512), one side of the fixed strip (511) away from the through hole (5113) is fixedly connected with a sliding bead (5112), the sliding bead (5112) is embedded and slides in the sliding rail (512), one side of the sliding rail (512) close to the fixed ball (513) is provided with an avoiding groove (5121) for clamping part of the fixed strip (511), the avoiding groove (5121) and the sliding groove of the sliding rail (512) are in communication with each other, and the number of the avoiding grooves (5121) is at least three and they are arranged in parallel with each other.

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