Method for in-situ polymerization of nano SiO2 nylon 1010 composite material and heating control equipment

Abstract

The invention belongs to the technical field of nano materials, and provides a method and heating control equipment for in-situ polymerization of a nano SiO2 nylon 1010 composite material, and the method comprises the following steps: S1, preparation of nylon salt, S2, preparation of a nano SiO2 / nylon 1010 composite molten material, and S3, preparation of composite material particles. And S2, adding the nylon salt containing 10-15% of ethanol, other ingredients and nano S O2 into a polymerization kettle according to a certain proportion in the process of S2, vacuumizing, performing nitrogen protection, pressurizing and heating until the nylon salt begins to melt, performing pressure-maintaining heating, dehydrating to normal pressure, and emptying. In the S1 process, heating control equipment is adopted to integrate the functions of a dissolving kettle and a neutralizing kettle, and a wall sleeve design with better heat exchange performance, a stirring device design and the like are provided. According to the invention, the mechanical property of nylon 1010 is improved, the space utilization rate of a workshop can be improved through the heating control equipment, the preparation efficiency of nylon salt is improved, and the preparation efficiency of a composite material is further improved.

Description

Technical Field

[0001] The invention belongs to the technical field of nano materials, and in particular relates to a method for in-situ polymerization of nano SiO2 nylon 1010 composite materials and a heating control device. Background Art

[0002] Nylon 1010 is made by polycondensation of sebacic acid. Sebacic acid and decanediamine are dissolved in ethanol in an equal molar ratio, and neutralized at 75°C under normal pressure to generate nylon 1010 salt. In the reactor of nylon 1010 salt, polycondensation is carried out at 240-260°C and 1.2-2.5Mpa to obtain nylon 1010. Nylon 1010 is widely used in many fields due to its unique properties. It is used in aviation, aerospace, machinery, power generation equipment, instrumentation, automobile and motorcycle parts, textiles, food, metallurgy, chemical industry, electronic appliances, oil and liquid transportation, cables, daily necessities and special film products.

[0003] At present, pure nylon 1010 materials still have obvious deficiencies in some mechanical properties, such as impact resistance and elongation at break, and there are also obvious limitations in the fields of its application. Therefore, modified nylon 1010 is now regarded as an important development direction to improve its impact resistance and elongation at break. Secondly, on the production line for generating nylon salt, the corresponding components are generally dissolved in a dissolving kettle first, and then the neutralization and titration reaction is carried out in a neutralizing kettle. Moreover, both the dissolving kettle and the neutralizing kettle need to provide steam to complete the heating control. However, this will prolong the reaction cycle and increase the space occupied by the workshop, increase space costs, equipment costs and management costs, and is not conducive to the quality improvement and efficiency improvement of the workshop. Summary of the invention

[0004] In view of the problems existing in the above-mentioned nylon 1010 and the deficiencies existing in the process equipment, the present invention proposes a method for in-situ polymerization of nano-SiO2 nylon 1010 composite materials which has a reasonable design and is beneficial to improving the mechanical properties of the material, and from the aspect of process equipment, proposes a heating control device for in-situ polymerization of nano-SiO2 nylon 1010 composite materials which can simplify the equipment flow and improve production efficiency.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is that the method for in-situ polymerization of nano-SiO2 nylon 1010 composite material provided by the present invention comprises the steps of: S1, preparation of nylon salt; S2, preparation of nano-SiO2 / nylon 1010 composite molten material; S3, preparation of nano-SiO2 / nylon 1010 composite material particles, characterized in that the specific steps are as follows:

[0006] S1-1, prepare a decanediamine ethanol solution by mixing the refined decanediamine with ethanol at a ratio of 1:2, and pump the solution into a high-level tank;

[0007] S1-2, adding sebacic acid to the heating control device, preparing a sebacic acid-ethanol mixed solution at a ratio of sebacic acid / ethanol = 1:5, turning on steam heating, starting stirring and heating to dissolve, and obtaining a sebacic acid-ethanol solution;

[0008] S1-3, the heating control device continues to perform steam heating and raises the temperature to 70°C, drops of decanediamine ethanol solution are added, and a neutralization reaction is carried out while stirring. The reaction temperature is controlled at 75-77°C, and the reaction is completed until the pH is 7-7.2, and the temperature is kept for 5 minutes;

[0009] S1-4, exhaust steam, pass cooling water into the heating control device to cool the material in the heating control device to 30-35°C and stir;

[0010] S1-5, introducing the material obtained in S1-4 into a centrifuge dryer for drying to obtain nylon salt containing 10-15% ethanol;

[0011] S2-1, add the nylon salt containing 10-15% ethanol obtained in S1-4, other ingredients and nano-SiO2 into the polymerization kettle in a certain proportion, and evacuate for about 20 minutes, with a vacuum degree of 740 mmHg;

[0012] S2-2, fill with nitrogen to 0.1Mpa, start heating the heat transfer oil to raise the temperature to 180±10℃, and the nylon salt begins to melt; as the temperature rises, the pressure rises to 1.1-1.2MPa, and the pressure is maintained; the temperature rises to 200-230℃, the pressure in the polymerization kettle is 1.1-1.2MPa, dehydrate to normal pressure, and vent for 1h;

[0013] S3-1. After venting, wait for the material to cool to 220°C, fill nitrogen into the polymerization kettle. The pressure of the polymerization kettle is determined by the viscosity of the material, 0.2-1MPa. Open the discharge valve, and the material flows out through the injection head to the water tank for cooling. Then, it is cut into 3×4mm particles by a pelletizer and dried to obtain composite material particles.

[0014] Preferably, the nano-SiO2 is dispersible silicon dioxide nano-powder, and the dispersible silicon dioxide nano-powder is silicon dioxide nano-particles developed by liquid phase in-situ surface modification technology.

[0015] A heating control device for in-situ polymerized nano-SiO2 nylon 1010 composite material, comprising a tank body, the bottom and top of the tank body are respectively provided with legs and a sealing cover, a discharge pipe is provided at the bottom center of the tank body, a power device and a plurality of feed pipes are provided on the sealing cover, a power output end of the power device extends into the interior of the tank body and is provided with a stirring device connected thereto in a transmission manner, a neutralizing liquid input device, a pH meter and a wall sleeve are also provided inside the tank body, and a steam pipe, a vent pipe and a water inlet pipe connected to the wall sleeve are provided at the bottom of the tank body and a water outlet pipe, the wall sleeve includes a cylindrical section corresponding to the inner side surface of the tank body and a conical section matched with the inner bottom surface of the tank body, the cylindrical section is provided with a plurality of wing-shaped sections connected thereto and extending toward the center of the tank body, the longitudinal section of the wing-shaped section is triangular, and an auxiliary stirring assembly is provided between adjacent wing-shaped sections, the stirring device includes a stirring shaft, the stirring shaft is provided with a shaft sleeve transmission-connected thereto, the shaft sleeve is provided with a plurality of butterfly plates distributed in a circular array, and the butterfly plate is provided with a plurality of swirl parts distributed along the length direction of the stirring shaft.

[0016] Preferably, the top of the tank body is a necking structure, a transition cone is provided between the side of the tank body and the necking structure, and a titration connecting tube orifice is provided on the transition cone.

[0017] Preferably, the neutralizing liquid input device comprises a plurality of immersed jet tubes corresponding one-to-one to the wing-shaped segments, the ends of the immersed jet tubes extending obliquely upward toward the location of the stirring device, the tops of the immersed jet tubes are provided with connecting tubes, the tops of all the connecting tubes are provided with an annular mother tube connected thereto, the tops of the annular mother tubes are provided with a collecting tube, and the collecting tubes are nested inside the titration connecting tube mouth.

[0018] Preferably, the immersed jet tube includes a head U-shaped section, which is clamped with the inclined surface of the wing-shaped section, and L-shaped sections are arranged on both sides of the head U-shaped section, and the L-shaped mouth of the L-shaped section faces upward, and the ends of the two L-shaped sections are connected by a tail U-shaped section, which is clamped with the inclined surface of the wing-shaped section, and the tail U-shaped section is provided with a jet straight tube section.

[0019] Preferably, the width of the wing-shaped section gradually narrows from the distal side of the tank body to the central side of the tank body, the top angle and bottom angle of the wing-shaped section are respectively connected with the cylindrical section and the conical section, and the side angle of the wing-shaped section is biased to a position below its center of gravity.

[0020] Preferably, the top and bottom of the butterfly plate are respectively provided with an upper sinking opening and a lower sinking opening, and the side of the butterfly plate facing the direction of the wall sleeve is provided with an L-shaped opening that cooperates with the wing-shaped section, and the L-shaped opening includes an upper opening edge and a lower opening edge, and the length of the upper opening edge is greater than the length of the lower opening edge.

[0021] Preferably, the upper edge and the lower edge are both provided with a plurality of teeth distributed at intervals.

[0022] Preferably, the fin plate is provided with a center-shaped hole for installing a swirl component, the swirl component comprises a swirl body, the side of the swirl body is provided with an annular positioning groove for clamping the center-shaped hole, the inner side of the swirl body is provided with a swirl hole, the swirl hole comprises two trumpet mouths, and the two trumpet mouths are transitioned by a cylindrical mouth.

[0023] Preferably, the auxiliary stirring assembly includes an inclined mounting seat, a mounting opening is provided at the center of the mounting seat, an inclined shaft is provided in the mounting opening, a stirring impeller is provided at the end of the inclined shaft, a rotating stirring profile of the stirring impeller is conical, a rotation positioning groove is provided on the side of the inclined shaft, and a positioning bolt that cooperates with the rotation positioning groove is provided on the mounting seat.

[0024] Compared with the prior art, the advantages and positive effects of the present invention are:

[0025] 1. The method for in-situ polymerization of nano-SiO2 nylon 1010 composite material provided by the present invention has little effect on the tensile strength of nylon 1010 after the addition of nano-SiO2, while the elongation at break and the impact strength are higher than those of pure nylon. When the nano-SiO2 content is 0.16%, the elongation at break is increased by 58.3%, and the impact strength increases with the increase of the nano-SiO2 content. Moreover, under the condition that the tensile strength does not decrease significantly, the impact resistance of the material is significantly improved. Furthermore, the surface-modified nano-SiO2 / nylon 1010 hybrid material is prepared by the in-situ polymerization method, and the mechanical properties are better than those of the traditional nylon 1010 material on the market. In addition, the amount of nano-material added by the in-situ polymerization method is greatly reduced, and the cost is greatly reduced.

[0026] 2. A heating control device for in-situ polymerized nano-SiO2 nylon 1010 composite materials, which integrates the functions of a dissolving kettle and a neutralizing kettle, improves the space utilization rate of a workshop, and the heat exchange range of its wall sleeve can effectively penetrate into the interior of the material, with good heat exchange efficiency (heating performance and cooling performance); the use of a stirring device and an auxiliary stirring component can effectively improve the mixing performance and neutralization efficiency of the material, which is beneficial to improving the preparation efficiency of nylon salt; the swirl element can form a local swirl inside the material during the stirring process of the stirring device, which can further improve the dissolution efficiency of the equipment; the use of an immersed jet tube as a burette can improve the mixing efficiency of the decanediamine ethanol solution and the raw material, thereby improving the neutralization efficiency of the equipment and reducing the waste of raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0028] Figure 1 The mechanical properties analysis table of the in-situ nylon 1010 material and the nano-SiO2 / nylon 1010 composite material prepared by the present invention;

[0029] Figure 2 It is a cross-sectional view of the heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material in the GG direction;

[0030] Figure 3 It is a front view of the heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material;

[0031] Figure 4 A side view of a heating control device for in-situ polymerized nano-SiO2 nylon 1010 composite material;

[0032] Figure 5 It is a cross-sectional view of the heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material in the EE direction;

[0033] Figure 6 A schematic diagram of the distribution of the wall sleeve and the auxiliary stirring assembly provided in the embodiment inside the tank body;

[0034] Figure 7 An axonometric view of the wall sleeve and the auxiliary stirring assembly provided in the embodiment inside the tank body;

[0035] Figure 8 An axonometric view of a stirring device provided in an embodiment;

[0036] Fig. 9 A cross-sectional view of an auxiliary stirring assembly provided in an embodiment;

[0037] Fig.10 An axonometric view of a neutralizing liquid input device provided in an embodiment;

[0038] Fig.11 A front view of a neutralizing liquid input device provided in an embodiment;

[0039] Fig.12 A top view of a swirl element provided in an embodiment;

[0040] Fig.13 A cross-sectional view of the swirl component provided in the embodiment along the FF direction.

[0041] In the above figures, 1, tank body; 11, discharge pipe; 12, steam pipe; 13, vent pipe; 14, water inlet pipe; 15, water outlet pipe; 16, wall sleeve; 161, columnar section; 162, conical section; 163, wing section; 17, titration connection pipe mouth; 2, support leg; 3, sealing cover; 31, feed pipe; 4, power device; 5, stirring device; 51, stirring shaft; 52, shaft sleeve; 53, butterfly plate; 531, upper sinking mouth; 532, lower sinking mouth; 533, L-shaped mouth; 534, tooth mouth; 535, middle-shaped hole; 6 , neutralizing liquid input device; 61, immersed jet tube; 611, head U-shaped section; 612, L-shaped section; 613, tail U-shaped section; 614, jet straight pipe section; 62, connecting pipe; 63, annular mother pipe; 64, collecting pipe; 7, auxiliary stirring assembly; 71, mounting seat; 72, mounting port; 73, inclined axis; 74, stirring impeller; 75, rotating positioning groove; 76, positioning bolt; 8, swirl part; 81, swirl body; 82, annular positioning groove; 83, swirl hole; 831, bell mouth; 832, cylindrical mouth. DETAILED DESCRIPTION

[0042] In order to more clearly understand the above-mentioned objects, features and advantages of the present invention, the present invention is further described below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict. For the convenience of description, if the words "upper", "lower", "left" and "right" appear below, they only indicate that the upper, lower, left and right directions are consistent with the accompanying drawings themselves, and do not limit the structure.

[0043] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways than those described herein. Therefore, the present invention is not limited to the specific embodiments of the following disclosure.

[0044] Embodiment: The method for in-situ polymerization of nano-SiO2 nylon 1010 composite material provided by the present invention comprises the steps of: S1, preparation of nylon salt; S2, preparation of nano-SiO2 / nylon 1010 composite molten material; S3, preparation of nano-SiO2 / nylon 1010 composite material particles, characterized in that: the specific steps are as follows:

[0045] S1-1, prepare a decanediamine ethanol solution by mixing the refined decanediamine with ethanol at a ratio of 1:2, and pump the solution into a high-level tank;

[0046] S1-2, adding sebacic acid to the heating control device, preparing a sebacic acid-ethanol mixed solution at a ratio of sebacic acid / ethanol = 1:5, turning on steam heating, starting stirring and heating to dissolve, and obtaining a sebacic acid-ethanol solution;

[0047] S1-3, the heating control device continues to perform steam heating and raises the temperature to 70°C, drops of decanediamine ethanol solution are added, and a neutralization reaction is carried out while stirring. The reaction temperature is controlled at 75-77°C, and the reaction is completed until the pH is 7-7.2, and the temperature is kept for 5 minutes;

[0048] S1-4, exhaust steam, pass cooling water into the heating control device to cool the material in the heating control device to 30-35°C and stir;

[0049] S1-5, introducing the material obtained in S1-4 into a centrifuge dryer for drying to obtain nylon salt containing 10-15% ethanol;

[0050] S2-1, add the nylon salt containing 10-15% ethanol obtained in S1-4, other ingredients and nano-SiO2 into the polymerization kettle in a certain proportion, and evacuate for about 20 minutes, with a vacuum degree of 740 mmHg;

[0051] S2-2, fill with nitrogen to 0.1Mpa, start heating the heat transfer oil to raise the temperature to 180±10℃, and the nylon salt begins to melt; as the temperature rises, the pressure rises to 1.1-1.2MPa, and the pressure is maintained; the temperature rises to 200-230℃, the pressure in the polymerization kettle is 1.1-1.2MPa, dehydrate to normal pressure, and vent for 1h;

[0052] S3-1. After venting, wait for the material to cool to 220°C, fill nitrogen into the polymerization kettle. The pressure of the polymerization kettle is determined by the viscosity of the material, 0.2-1MPa. Open the discharge valve, and the material flows out through the injection head to the water tank for cooling. Then, it is cut into 3×4mm particles by a pelletizer and dried to obtain composite material particles.

[0053] The nano-SiO2 is a dispersible silicon dioxide nano-powder, which is a silicon dioxide nano-particle developed by using liquid phase in-situ surface modification technology.

[0054] like Figure 1 As shown in the figure, the relationship between the mechanical properties of in-situ nylon 1010 composite materials and the nano-SiO2 content is listed. The addition of nano-SiO2 has little effect on the tensile strength of nylon 1010, while the elongation at break and impact strength are higher than those of pure nylon. When the nano-SiO2 content is 0.16%, the elongation at break increases by 58.3%, the impact strength increases with the increase of nano-SiO2 content, and the impact resistance is also good.

[0055] Furthermore, the nano-SiO2 provided by the process of the present invention is developed by using the liquid phase in-situ surface modification technology. This technology is to modify the surface of the nano-SiO2 with organic compounds to achieve controllable particle size when the nano-particles are initially generated, and at the same time give the nano-particles some special properties. The structure is designable, and different methods can be used to prepare silicon dioxide nano-particles for different purposes and specifications. It can also be made to have special functional groups on its surface and well dispersed in special media according to different usage requirements. Dispersible silicon dioxide nano-particles are divided into two series: NLN series and NLR series. Among them, the NLN series is nano-silicon dioxide modified with saturated organic carbon chains or polymers; the NLR series is nano-silicon dioxide particles with organic chains or reactive functional groups (such as double bonds, amino groups, hydroxyl groups, epoxy groups, mercapto groups, etc.) on the surface, which can continue to participate in various organic reactions and polymer polymerization reactions, so that the nano-particles have better bonding strength with the matrix material. By adopting the dispersible silicon dioxide nanopowder in the present invention and using a silicon oxide mass fraction far lower than that in melt blending (lower than 1 / 10), the purpose and index of significantly improving the impact resistance of the material can be achieved without significantly decreasing the tensile strength. The amount of nanomaterial added by the in-situ polymerization method is greatly reduced, and the cost is greatly reduced.

[0056] like Figures 2 to 13 As shown, a heating control device for an in-situ polymerized nano-SiO2 nylon 1010 composite material provided by the present invention comprises a tank body 1, the bottom and top of the tank body 1 are respectively provided with legs 2 and a sealing cover 3, a discharge pipe 11 is provided at the bottom center of the tank body 1, a power device 4 and a plurality of feed pipes 31 are provided on the sealing cover 3, a power output end of the power device 4 extends into the interior of the tank body 1 and is provided with a stirring device 5 connected thereto in a transmission manner, a neutralizing liquid input device 6, a pH meter (not shown) and a wall sleeve 16 are further provided inside the tank body 1, and a steam pipe 12, a vent pipe 13, a water inlet pipe 14 and a water outlet pipe 15 connected to the wall sleeve 16 are provided at the bottom of the tank body 1. Among them, the tank body 1, the support legs 2, the sealing cover 3, the discharge pipe 11, the power device 4, the feed pipe 31, the steam pipe 12, the vent pipe 13, the pH meter, the water inlet pipe 14 and the water outlet pipe 15 are prior arts, wherein the steam pipe 12 is used to heat the steam into the wall sleeve 16 when the material needs to be heated, and the water inlet pipe 14 and the water outlet pipe 15 are used to cool the mixed solution of nylon salt in the S1-4 process, and corresponding control valves are arranged on the feed pipe 31, the steam pipe 12, the vent pipe 13, the water inlet pipe 14 and the water outlet pipe 15 for controlling the inlet and outlet flow rates and the steam inlet and outlet flow rates, which will not be described in detail in this embodiment.

[0057] In order to improve the utilization rate of the present equipment, the wall sleeve 16 provided by the present invention includes a cylindrical section 161 corresponding to the inner side surface of the tank body 1 and a conical section 162 matched with the inner bottom surface of the tank body 1, and the cylindrical section 161 is provided with a plurality of wing-shaped sections 163 connected thereto and extending toward the center direction of the tank body 1, and the longitudinal section of the wing-shaped section 163 is triangular, and an auxiliary stirring assembly 7 is arranged between adjacent wing-shaped sections 163, and the stirring device 5 includes a stirring shaft 51, and the stirring shaft 51 is provided with a shaft sleeve 52 which is transmission-connected thereto, and the shaft sleeve 52 is provided with a plurality of butterfly plates 53 distributed in a circular array, and the butterfly plate 53 is provided with a plurality of swirl parts 8 distributed along the length direction of the stirring shaft 51. This equipment combines the functions of a dissolving kettle and a neutralizing kettle, improves the space utilization rate of the workshop, and its wall sleeve 16, in addition to having a cylindrical section 161 and a conical section 162 to hold and heat the entire material, also designs a wing-shaped section 163 to effectively extend the heat exchange range into the interior of the material, which can effectively improve the heat exchange efficiency (heating performance and cooling performance) of this equipment. Furthermore, in coordination with the stirring device 5, the present invention designs an auxiliary stirring component 7, and uses the power transmitted by the stirring device 5 to drive the auxiliary stirring component 7 to generate a rotating power, thereby allowing the material to be fully stirred at a position close to the wing-shaped section 163, and the material between adjacent wing-shaped sections 163 will also produce repeated collisions under the action of high-speed stirring, while causing the auxiliary stirring component 7 to perform a stirring action, improving the effective collision between material molecules, thereby improving the dissolution efficiency and neutralization efficiency of the material, which is beneficial to improving the preparation efficiency of nylon salt.

[0058] Furthermore, the stirring device 5 provided by the present invention adopts a butterfly plate 53 matched with the design of the wing-shaped section 163 as a stirring actuator. The stirring range generated by the butterfly plate 53 rotating continuously with the stirring device 5 just avoids the extension range of the wing-shaped section 163, and leaves space for secondary stirring for the materials between the wing-shaped sections 163, which is also convenient for the materials after secondary stirring to continue to participate in the materials within the range of the butterfly plate 53. At the same time, during the stirring process of the stirring device 5, the swirl element 8 can generate a spiral pulling force after a part of the material passes through the swirl element 8 at high speed, thereby forming a local swirl inside the material, further improving the dissolution efficiency and neutralization efficiency of the material in the tank body 1, and to a certain extent, it also reduces the heating time and the supply of steam, which meets the requirements of improving quality and efficiency. The present invention uses an immersed jet tube 61 as a burette, and ejects the decanediamine ethanol solution toward the stirring center of the material by jetting from the inside of the material, so that the decanediamine ethanol solution is mixed with the movement of the material, which is conducive to improving the neutralization efficiency of the equipment and reducing the waste of raw materials.

[0059] In order to facilitate the provision of decanediamine ethanol solution to the interior of the tank body 1 to achieve the neutralization reaction of the nylon salt solution, the top of the tank body 1 is designed as a necking structure in the present invention, and a transition cone is provided between the side of the tank body 1 and its necking structure, and a titration connecting pipe mouth 17 is provided on the transition cone. The titration connecting pipe mouth 17 is used to provide an input node to the neutralization liquid input device 6, avoiding the feeding direction of the feed pipe 31 and the stirring working surface of the stirring device 5.

[0060] In order to improve the neutralization efficiency in the process of preparing nylon salt by the equipment, the neutralization liquid input device 6 provided by the present invention includes a plurality of immersed jet tubes 61 corresponding one by one to the wing-shaped sections 163, and the ends of the immersed jet tubes 61 extend obliquely upward toward the location of the stirring device 5. A connecting tube 62 is arranged on the top of the immersed jet tube 61, and an annular mother tube 63 connected thereto is arranged on the top of all the connecting tubes 62. A collecting pipe 64 is arranged on the top of the annular mother tube 63, and the collecting pipe 64 is nested inside the titration connecting pipe mouth 17. Among them, the immersed jet tube 61 is mounted on the wing section 163 in a riding manner, and all the immersed jet tubes 61 use the connecting tube 62 as a branch pipe to establish a branch relationship with the annular mother pipe 63. The collecting pipe 64 and the annular mother pipe 63 uniformly provide the prepared decanediamine ethanol solution to the immersed jet tube 61. The decanediamine ethanol solution is finally ejected from the immersed jet tube 61 to the center of the stirring range formed by the stirring device 5, thereby realizing the neutralization process of the acid and alkali liquid, shortening the reaction time of the solution, and improving the efficiency of the neutralization reaction, thereby shortening the process of reaching the standard of the real-time pH value detected by the pH meter, thereby reducing the continued supply of decanediamine ethanol solution, which is beneficial to accurately control the quality of the nylon salt solution.

[0061] Matching with the wing-shaped section 163, the immersed jet tube 61 provided by the present invention includes a head U-shaped section 611, the head U-shaped section 611 is clamped with the inclined surface of the wing-shaped section 163, L-shaped sections 612 are arranged on both sides of the head U-shaped section 611, the L-shaped opening 533 of the L-shaped section 612 faces upward, the ends of the two L-shaped sections 612 are connected by a tail U-shaped section 613, the tail U-shaped section 613 is clamped with the inclined surface of the wing-shaped section 163, and the tail U-shaped section 613 is provided with a jet straight tube section 614. In this way, in addition to establishing a relatively stable assembly relationship with the wing-shaped section 163 by means of a fork, the ethanol solution of decanediamine as a titration liquid can generate heat exchange with the wing-shaped section 163 during the ejection process, thereby reducing the temperature difference between the ethanol solution of decanediamine and the material in the tank body 1, improving the mixing effect and neutralization efficiency of the ethanol solution of decanediamine and the material, and thus improving the production efficiency of the present equipment.

[0062] In order to improve the heat exchange efficiency between the wing-shaped section 163 and the material, the width of the wing-shaped section 163 provided by the present invention gradually narrows from the distal side of the tank body 1 to the central side of the tank body 1, the top angle and bottom angle of the wing-shaped section 163 are respectively connected with the cylindrical section 161 and the conical section 162, and the side angle of the wing-shaped section 163 is biased to a position below its center of gravity. In this way, the gradual width design of the wing-shaped section 163 is conducive to the flow of materials toward the stirring center of the stirring device 5; the plate surface of the wing-shaped section 163 can directly exchange heat with the material, and the position design of the side angle of the wing-shaped section 163 leaves sufficient space for the material to rotate with the stirring device 5; and according to the principle of heat rising, the heat in the wing-shaped section 163 can heat the material from bottom to top, thereby improving the heating efficiency of the material inside the device during the heating stage.

[0063] In order to improve the stirring efficiency of the stirring device 5 during steps S1-2 and S1-3, the top and bottom of the butterfly plate 53 provided by the present invention are respectively provided with an upper sinking opening 531 and a lower sinking opening 532, and the side of the butterfly plate 53 facing the direction of the wall sleeve 16 is provided with an L-shaped opening 533 matched with the wing-shaped section 163, and the L-shaped opening 533 includes an upper opening edge and a lower opening edge, and the length of the upper opening edge is greater than the length of the lower opening edge. Further, a plurality of tooth openings 534 are arranged at intervals on both the upper opening edge and the lower opening edge. Among them, the design of the upper sinking mouth 531 and the lower sinking mouth 532 provides an effective passage path for the material, so that the material can produce appropriate tumbling within the stirring range, especially when the material level is higher than the butterfly plate 53, increasing the number of collisions between the material molecules; the L-shaped mouth 533 cooperates with the side angle of the wing-shaped section 163 to form a reasonable stirring range, and the tooth mouth 534 is used to subdivide and comb the rotating material, so that the material produces different rotation speeds locally, thereby improving the stirring efficiency of the equipment for the material, so as to shorten the actual time required for the dissolution process and the neutralization process.

[0064] In order to improve the swirl effect of the fin plate, the present invention is provided with a Chinese-character hole on the fin plate for installing the swirl member 8. The swirl member 8 includes a swirl body 81. The side of the swirl body 81 is provided with an annular positioning groove 82 connected to the Chinese-character hole. The inner side of the swirl body 81 is provided with a swirl hole 83. The swirl hole 83 includes two bell mouths 831. The two bell mouths 831 are transitioned through a cylindrical mouth 833. In the direction of continuous rotation of the material, the distributed material enters the swirl body 81 from the bell mouth 831. Due to the pressure difference between the front and rear pressures of the two bell mouths 831, coupled with the rotation of the swirl member 8, a fluid with a certain twisting tendency can be formed at the moment of extrusion from the other bell mouth 831, thereby improving the mixing efficiency inside the material.

[0065] In order to improve the utilization rate of the auxiliary stirring device 5, the auxiliary stirring assembly 7 provided by the present invention includes an inclined mounting seat 71, a mounting opening 72 is provided at the center of the mounting seat 71, an end cover is provided at the end of the mounting opening 72, an inclined shaft 73 penetrating the end cover is provided in the mounting opening 72, a bearing bushing that is rotatably matched with the inclined shaft 73 is provided between the end cover and the mounting seat 71, a stirring impeller 74 is provided at the end of the inclined shaft 73, the rotating stirring profile of the stirring impeller 74 is conical, a rotating positioning groove 75 is provided on the side of the inclined shaft 73, and a positioning bolt 76 that is matched with the rotating positioning groove 75 is provided on the mounting seat 71. In this way, the positioning bolt 76 and the rotating positioning groove 75 can generate a fixed rotating trajectory, so that the stirring impeller 74 has a determined rotating path, and the stirring impeller 74 can rotate by itself under the pressure of the material, and then react to the material to stir the material, and its conical rotating profile can make the material close to its rotation center quickly rush into the stirring range of the stirring device 5, thereby causing secondary stirring of the surrounding materials, thereby improving the stirring efficiency of the device. In particular, the rotating volume of the stirring fluid caused by the stirring device 5 at the bottom of the wing section 163 is smaller than the volume of the upper part of the wing section 163, and the stirring center of the auxiliary stirring component 7 is inclined downward, which can also reduce the resistance of the secondary stirred material entering the stirring range formed by the stirring device 5.

[0066] The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content disclosed above to change or modify it into an equivalent embodiment with equivalent changes and apply it to other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A method for in-situ polymerization of nano-SiO2 nylon 1010 composite material, comprising the steps of: S1, preparation of nylon salt; S2, preparation of nano-SiO2 / nylon 1010 composite molten material; S3, preparation of nano-SiO2 / nylon 1010 composite material particles, characterized in that: The specific steps are as follows: S1-1, prepare a decanediamine ethanol solution by mixing the refined decanediamine with ethanol at a ratio of 1:2, and pump the solution into a high-level tank; S1-2, adding sebacic acid to the heating control device, preparing a sebacic acid-ethanol mixed solution at a ratio of sebacic acid / ethanol = 1:5, turning on steam heating, starting stirring and heating to dissolve, and obtaining a sebacic acid-ethanol solution; S1-3, the heating control device continues to perform steam heating and raises the temperature to 70°C, drops of decanediamine ethanol solution are added, and a neutralization reaction is carried out while stirring. The reaction temperature is controlled at 75-77°C, and the reaction is completed until the pH is 7-7.2, and the temperature is kept for 5 minutes; S1-4, exhaust steam, pass cooling water into the heating control device to cool the material in the heating control device to 30-35°C and stir; S1-5, introducing the material obtained in S1-4 into a centrifuge dryer for drying to obtain nylon salt containing 10-15% ethanol; S2-1, add the nylon salt containing 10-15% ethanol obtained in S1-4, other ingredients and nano-SiO2 into the polymerization kettle in a certain proportion, and evacuate for about 20 minutes, with a vacuum degree of 740 mmHg; S2-2, fill with nitrogen to 0.1Mpa, start heating the heat transfer oil to raise the temperature to 180±10℃, and the nylon salt begins to melt; as the temperature rises, the pressure rises to 1.1-1.2MPa, and the pressure is maintained; the temperature rises to 200-230℃, the pressure in the polymerization kettle is 1.1-1.2MPa, dehydrate to normal pressure, and vent for 1h; S3-1. After venting, wait for the material to cool to 220°C, fill nitrogen into the polymerization kettle. The pressure of the polymerization kettle is determined by the viscosity of the material, 0.2-1MPa. Open the discharge valve, and let the material flow out through the injection head to the water tank for cooling. Then, it is cut into 3×4mm particles by a pelletizer and dried to obtain composite material particles.

2. The method for in-situ polymerization of nano-SiO2 nylon 1010 composite material according to claim 1, characterized in that: The nano-SiO2 is a dispersible silicon dioxide nano-powder, which is a silicon dioxide nano-particle developed by using liquid phase in-situ surface modification technology.

3. A heating control device for in-situ polymerized nano-SiO2 nylon 1010 composite material, comprising a tank body, the bottom and top of the tank body are respectively provided with legs and a sealing cover, a discharge pipe is provided at the bottom center of the tank body, a power device and a plurality of feed pipes are provided on the sealing cover, the power output end of the power device extends into the interior of the tank body and is provided with a stirring device connected thereto in a transmission manner, a neutralizing liquid input device, a pH meter and a wall sleeve are also provided inside the tank body, a steam pipe, a vent pipe, a water inlet pipe and a water outlet pipe connected to the wall sleeve are provided at the bottom of the tank body, characterized in that: The wall sleeve includes a cylindrical section corresponding to the inner side surface of the tank body and a conical section matched with the inner bottom surface of the tank body. The cylindrical section is provided with a plurality of wing-shaped sections connected with it and extending toward the center direction of the tank body. The longitudinal section of the wing-shaped section is triangular, and an auxiliary stirring assembly is arranged between adjacent wing-shaped sections. The stirring device includes a stirring shaft, and the stirring shaft is provided with a shaft sleeve connected to the stirring shaft for transmission. The shaft sleeve is provided with a plurality of butterfly plates distributed in a circular array, and the butterfly plate is provided with a plurality of swirl parts distributed along the length direction of the stirring shaft.

4. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 3 is characterized in that: The top of the tank body is a necking structure, a transition cone surface is arranged between the side of the tank body and the necking structure, and a titration connecting tube orifice is arranged on the transition cone surface.

5. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 4, characterized in that: The neutralizing liquid input device includes a plurality of immersed jet tubes corresponding one by one to the wing-shaped segments, the ends of the immersed jet tubes extending obliquely upward toward the location of the stirring device, the tops of the immersed jet tubes are provided with connecting tubes, the tops of all the connecting tubes are provided with an annular mother tube connected thereto, the tops of the annular mother tubes are provided with a collecting tube, and the collecting tubes are nested inside the titration connecting tube opening.

6. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 5, characterized in that: The immersed jet tube includes a head U-shaped section, which is clamped with the inclined surface of the wing-shaped section. L-shaped sections are arranged on both sides of the head U-shaped section, and the L-shaped openings of the L-shaped sections face upward. The ends of the two L-shaped sections are connected by a tail U-shaped section, which is clamped with the inclined surface of the wing-shaped section. The tail U-shaped section is provided with a jet straight tube section.

7. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 1, characterized in that: The width of the wing-shaped section gradually narrows from the distal side of the tank body to the central side of the tank body, the top angle and bottom angle of the wing-shaped section are respectively connected with the columnar section and the conical section, and the side angle of the wing-shaped section is biased to a position below its center of gravity.

8. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 7, characterized in that: The top and bottom of the butterfly plate are respectively provided with an upper sinking mouth and a lower sinking mouth, and the side of the butterfly plate facing the direction of the wall sleeve is provided with an L-shaped mouth that cooperates with the wing-shaped section, and the L-shaped mouth includes an upper mouth edge and a lower mouth edge, and the length of the upper mouth edge is greater than the length of the lower mouth edge, and the upper mouth edge and the lower mouth edge are both provided with a plurality of spaced teeth.

9. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 3 or 8, characterized in that: The fin plate is provided with a Chinese-character hole for installing a swirl component, the swirl component includes a swirl body, the side of the swirl body is provided with an annular positioning groove engaged with the Chinese-character hole, the inner side of the swirl body is provided with a swirl hole, the swirl hole includes two trumpet mouths, and the two trumpet mouths are transitioned by a cylindrical mouth.

10. The heating control device of the in-situ polymerized nano-SiO2 nylon 1010 composite material according to claim 3, characterized in that: The auxiliary stirring assembly includes an inclined mounting seat, a mounting opening is provided at the center of the mounting seat, an inclined shaft is provided in the mounting opening, a stirring impeller is provided at the end of the inclined shaft, a rotating stirring profile of the stirring impeller is conical, a rotation positioning groove is provided on the side of the inclined shaft, and a positioning bolt that cooperates with the rotation positioning groove is provided on the mounting seat.

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