Low-freezing-point production system and method of methyltriacetoxysilane

Abstract

The invention discloses a low-freezing-point production system and method for methyltriacetoxysilane, and belongs to the technical field of methyltriacetoxysilane preparation.The low-freezing-point production system for methyltriacetoxysilane comprises a pretreatment module, a condensation module and a condensation module, the pretreatment module comprises a premixing tank, and the premixing tank is used for premixing raw materials; the reaction module comprises a reaction tank and a replacement part, the replacement part is arranged on the reaction tank and can be communicated with an inner cavity of the reaction tank, the premixing tank is connected with the replacement part through a pipeline, and the premixed raw materials enter the reaction tank through the replacement part; and when the dynamic copolymerization reaction is carried out in the reaction tank, nitrogen is introduced into the reaction tank through the replacement part to replace air in the reaction tank. Integration is achieved, and multiple function requirements are met; in addition, low-freezing-point production of methyltriacetoxysilane is realized through a series of steps such as air replacement during dynamic copolymerization.

Description

Technical Field

[0001] The invention relates to the technical field of methyltriacetoxysilane preparation, in particular to a low-freezing-point production system and method for methyltriacetoxysilane. Background Art

[0002] In the production of methyltriacetoxysilane, raw material premixing and reaction are crucial. In traditional processes, raw materials are premixed and transferred to a reaction tank for reaction. Nitrogen is introduced to displace the air to prevent side reactions and ensure reaction stability. However, existing production systems have significant flaws. Liquid injection and air replacement are often completed through multiple connectors, lacking an integrated design. This makes the operation cumbersome and error-prone, making precise control difficult and easily leading to air intrusion, which affects product quality and yield.

[0003] Furthermore, the high freezing point of methyltriacetoxysilane limits its application and storage performance. Conventional production methods struggle to effectively lower the freezing point, making it difficult to meet market demand for high-performance, low-freeze-point products. Therefore, developing an integrated, multifunctional low-freeze-point production system and method to achieve efficient production and improved performance has become a key issue in this field. Summary of the Invention

[0004] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid obscuring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.

[0005] In view of the above problems and / or the problems existing in the prior art, the present invention is proposed.

[0006] Therefore, the first object of the present invention is to provide a low freezing point production system for methyltriacetoxysilane, which is integrated and meets multiple functions.

[0007] In order to solve the above technical problems, the present invention provides the following technical solutions: a low-freezing-point production system for methyltriacetoxysilane, comprising a pretreatment module, including a premixing tank, which is used for premixing raw materials; a reaction module, including a reaction tank and a displacement piece, which is arranged on the reaction tank and can be communicated with the inner cavity of the reaction tank, the premixing tank is connected to the displacement piece through a pipeline, and the premixed raw materials enter the reaction tank through the displacement piece; and when a dynamic copolymerization reaction is carried out in the reaction tank, nitrogen is passed into the reaction tank through the displacement piece to replace the air in the reaction tank.

[0008] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, the replacement part includes a mounting shell and an injection tube, and the injection tube is used to inject liquid or gas into the reaction tank; the mounting shell is arranged on the reaction tank, and the injection tube is inserted into the mounting shell, and the injection tube is elastically connected to the mounting shell, and the injection tube can move in the axial direction relative to the mounting shell.

[0009] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, a transition cavity is provided inside the mounting shell, and the contour shape of the end of the injection tube located inside the mounting shell can match the contour shape of the transition cavity.

[0010] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, the bottom of the mounting shell is provided with a mounting hole, the mounting hole is connected to the transition chamber, a first floating piece is elastically installed in the mounting hole, and a first channel is also opened at the bottom of the mounting shell, the first channel is connected to the mounting hole, and the first floating piece switches the conductive or blocked state between the first channel and the transition chamber by floating itself.

[0011] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, wherein: a second channel is further opened at the bottom of the installation shell, and the second channel is connected to the transition chamber; When the displacement part is used to inject liquid into the reaction tank, the injection tube floats up due to the liquid level until the second channel also flows liquid; when the displacement part is used to inject nitrogen into the reaction tank, the injection tube is stationary relative to the mounting shell, and the second channel is used to discharge the displaced air in the reaction tank.

[0012] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, a third channel is provided on the injection tube, the third channel is used to connect the transition chamber and the outside of the reaction tank, and the displaced air in the reaction tank is discharged through the second channel and the third channel.

[0013] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, a second floating plate is elastically installed in the third channel, and the second floating plate is pushed by the displaced air to switch the conductive state between the transition chamber and the outside of the reaction tank.

[0014] As a preferred solution of the low-freezing-point production system of methyltriacetoxysilane of the present invention, the first channel is arranged obliquely, and the extension line of the first channel intersects with the central axis of the installation shell.

[0015] The second object of the present invention is to provide a method for producing methyltriacetoxysilane at a low freezing point. The method includes adding raw materials methyltrichlorosilane and ethyltriacetoxysilane into a premixing tank for premixing; transferring the raw materials after premixing to a reaction tank, and dynamically copolymerizing methyltrichlorosilane and ethyltriacetoxysilane under the action of a composite catalyst, during which nitrogen is passed through a displacement piece to replace air; adding a sustained-release agent and controlling the release through ultrasound; and synergistically inhibiting crystallization through gradient cooling and ultrasound.

[0016] As a preferred embodiment of the low-freezing-point production method of methyltriacetoxysilane of the present invention, the composite catalyst comprises HMPA and nano-titanium dioxide-supported phosphazene in a mass ratio of 4:1; and the cooling rate of the gradient cooling is controlled at 5°C / h in the 60-40°C stage and 1°C / h in the 40-20°C stage.

[0017] The beneficial effects of the present invention are as follows: the present invention injects liquid into the reaction tank through the displacement part, and can also use the displacement part to replace the air in the reaction tank during the dynamic copolymerization reaction in the reaction tank, thereby achieving integration and meeting multiple functional requirements; in addition, through a series of steps such as replacing air during the dynamic copolymerization reaction, the low-freezing point production of methyltriacetoxysilane is achieved. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be derived from these drawings without inventive effort. Among them: Figure 1 This is a wiring diagram of a low-freezing-point production system for methyltriacetoxysilane.

[0019] Figure 2 Schematic diagram of the replacement part for the low-freezing-point production system for methyltriacetoxysilane.

[0020] Figure 3 A top view of a replacement part for a low-freezing-point production system for methyltriacetoxysilane.

[0021] Figure 4 Axonometric view of a replacement part for a low-freezing-point production system for methyltriacetoxysilane.

[0022] Figure 5 A cross-sectional view of a replacement part for a low-freezing-point production system for methyltriacetoxysilane.

[0023] Figure 6 This is a cross-sectional view of a displacement component during injection of a low-freezing-point production system for methyltriacetoxysilane.

[0024] Figure 7 Cross-sectional view of a displacement component during nitrogen injection in a low-freezing-point production system for methyltriacetoxysilane. DETAILED DESCRIPTION

[0025] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below with reference to the accompanying drawings.

[0026] 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 different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0027] Next, the present invention is described in detail with reference to schematic diagrams. For ease of illustration, when describing embodiments of the present invention, cross-sectional views illustrating device structures may be partially enlarged and not to scale. Furthermore, these schematic diagrams are merely illustrative and should not limit the scope of protection of the present invention. Furthermore, in actual production, three-dimensional dimensions, including length, width, and depth, should be included.

[0028] Furthermore, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments. Example 1

[0029] Reference Figure 1 , which is the first embodiment of the present invention, provides a low-freezing point production system for methyltriacetoxysilane, including a pretreatment module 1 and a reaction module 2.

[0030] Specifically, the pretreatment module 1 includes a premixing tank 11, which is used for premixing raw materials. The raw materials are methyltrichlorosilane and ethyltriacetoxysilane. The raw materials are added to the premixing tank 11 through a pipeline for heating and premixing.

[0031] Preferably, the reaction module 2 includes a reaction tank 21 and a displacement piece 22, the premixing tank 11 is connected to the displacement piece 22 through a pipeline, and the premixed raw materials enter the reaction tank 21 for the next reaction; wherein, the displacement piece 22 is arranged on the reaction tank 21, and the displacement piece 22 connecting pipeline is connected to the inner cavity of the reaction tank 21, that is, the premixed raw materials enter the reaction tank 21 through the displacement piece 22; when a dynamic copolymerization reaction is carried out in the reaction tank 21, it is necessary to replace the air in the reaction tank 21, and the displacement piece 22 is used to replace the air in the reaction tank 21 while passing nitrogen into the reaction tank 21, and the air in the reaction tank 21 is discharged through the displacement piece 22.

[0032] By integrating the design of the replacement part 22 of the pretreatment module 1 and the reaction module 2, the integrated operation of raw material premixing and nitrogen replacement is achieved, which reduces the complexity of the equipment and the operation steps, avoids side reactions caused by air mixing, and improves the stability of the reaction system. Example 2

[0033] See Figures 1 to 7 , which is the second embodiment of the present invention, is based on embodiment 1.

[0034] Specifically, the displacement member 22 includes a mounting shell 221 and an injection tube 222. The mounting shell 221 is disposed on the reaction tank 21 and is used to mount the injection tube 222. The injection tube 222 is inserted into the mounting shell 221 and is elastically connected to the mounting shell 221. In this embodiment, a spring is provided at the top of the mounting shell 221, which contacts the bottom wall of the top of the injection tube 222. When the injection tube 222 undergoes axial displacement relative to the mounting shell 221, the spring is used to reset the injection tube 222. The injection tube 222 is connected to a pipeline, and different pipelines and the injection tube 222 are used to inject liquid or gas into the reaction tank 21. The elastic connection between the injection tube 222 and the mounting shell 221 can automatically adjust the reset of the injection tube 222 after the medium liquid is injected. At the same time, it can ensure the sealing during liquid injection and smooth exhaust during gas replacement, thereby improving operational flexibility and safety.

[0035] Preferably, a transition cavity 221a is provided within the mounting shell 221, and the contour of the end portion of the injection tube 222 located within the mounting shell 221 is adapted to mate with and conform to the contour of the transition cavity 221a. In this embodiment, the cross-sectional shape of the transition cavity 221a is an isosceles trapezoid, wherein the length of the lower base is shorter than the length of the upper base. The cross-sectional shape of the lower end portion of the injection tube 222 is also an isosceles trapezoid. The conforming design of the injection tube 222 to the contour of the transition cavity 221a reduces the risk of leakage during gas injection and ensures efficient medium transmission.

[0036] Preferably, the bottom of the mounting shell 221 is provided with a mounting hole 221b, coaxially arranged with the mounting shell 221 and communicating with the transition chamber 221a. A first floating plate 223 is elastically mounted within the mounting hole 221b via a spring. When pressed, the first floating plate 223 can move downward along the axial direction of the mounting hole 221b. The bottom of the mounting shell 221 also defines a first channel 221c, communicating with the mounting hole 221b. The first floating plate 223 floats to switch between a conductive and blocked state between the first channel 221c and the transition chamber 221a. The first channel 221c is tilted, with its extension intersecting the central axis of the mounting shell 221. This tilted design, combined with the smaller inner diameter of the first channel 221c, creates a mist-like spray pattern and allows for a wider dispersion range. Furthermore, the floating first floating plate 223 provides a second safety feature to prevent misoperation.

[0037] Preferably, the bottom of the mounting shell 221 is further provided with a second channel 221d, which communicates with the transition chamber 221a. Three second channels 221d are provided, evenly spaced around the circumference of the mounting shell 221. When the displacer 22 is used to inject liquid into the reaction tank 21, due to the limited discharge speed, the injection tube 222 is lifted by the liquid level until the second channel 221d also circulates liquid, allowing the first channel 221c and the second channel 221d to circulate liquid simultaneously, ensuring uniform distribution while improving injection efficiency. When the displacer 22 is used to inject nitrogen into the reaction tank 21, the injection tube 222 is stationary relative to the mounting shell 221, while the second channel 221d is used to exhaust the displaced air in the reaction tank 21. The second channel circulates liquid during injection and exhausts air during displacement, achieving multifunctional integration in a single device, simplifying piping design, and reducing equipment costs.

[0038] Furthermore, a third channel 222a is provided on the injection tube 222, and the third channel 222a is used to connect the transition chamber 221a and the outside of the reaction tank 21. In this embodiment, three third channels 222a are provided, and the three third channels 222a are evenly arranged in the circumferential direction of the injection tube 222. The displaced air in the reaction tank 21 is discharged through the second channel 221d and the third channel 222a, so that the displacement part 22 can inject nitrogen and discharge air at the same time.

[0039] Furthermore, a second floating plate 224 is elastically mounted within the third channel 222a. This plate is pushed by the displaced air to switch the flow between the transition chamber 221a and the exterior of the reaction tank 21. When the displacer 22 is being filled with liquid, the second floating plate 224 closes the third channel 222a, preventing liquid from flowing into it. The combination of the third channel 222a and the second floating plate 224 ensures efficient exhaust of displaced air, preventing pressure imbalance within the reaction tank 21 and ensuring a stable reaction process. Example 3

[0040] This is the third embodiment of the present invention, which provides a method for producing methyltriacetoxysilane at a low freezing point. The method comprises the following steps: S101: Add methyltrichlorosilane and ethyltriacetoxysilane in a molar ratio of 7:3 to premix tank 11 and preheat to 40°C; add microencapsulated silane sustained-release agent (10% of the total silane mass) and stir at 300 rpm for 15 minutes. After premixing, transfer the raw materials to reaction tank 21; S102: Ultrasonic treatment (20 kHz, 500 W) was applied for 20 minutes to destroy the PDMS shell and release 20% methyltrimethoxysilane into the system; S201: Add composite catalyst (1.2% of the total reactant mass, including HMPA and nano-phosphazene mass ratio of 4:1), and replace the air with nitrogen.

[0041] S202: Three-stage temperature rise reaction: Stage A (55°C): Maintain for 1 hour, initial esterification reaction (conversion rate 60%-70%); Stage B (60°C): Increase the pressure to 0.12 MPa, react for 1.5 hours, and the conversion rate reaches 95%; Stage C (50°C): reduce the pressure to normal pressure and continue the reaction for 0.5 hours, with a total reaction time of 3 hours; S301: Add magnetic nano-alumina (sodium methoxide loading 20%) to the reaction solution at a molar ratio of HCl:sodium methoxide = 1:1.05; S302: Turn on the magnetic field (0.5 T) to adsorb the aluminum oxide particles, and the liquid phase is extracted through a filter membrane (0.22 μm). After neutralization, the pH value is 6.8 ± 0.2; S401: distillation temperature 90°C, vacuum degree 0.8 kPa, collecting the 108-110°C fraction (purity 99.5%); S402: Dynamic crystallization control: 60℃→40℃: cooling rate 5℃ / h, ultrasonic intermittent start (5 minutes on / 10 minutes off); 40℃→20℃: cooling rate 1℃ / h, continuous ultrasonic operation (power 300 W); S501: Plasticizer blending: Add bio-based plasticizer (polyether-modified silicone oil, 5 wt%) and shear stir at 400 rpm at 50°C for 1 hour.

[0042] This invention incorporates ethyltriacetoxysilane and a microencapsulated sustained-release agent to disrupt molecular symmetry, lower the freezing point, and extend storage stability. The composite catalyst (HMPA + nano-phosphazene) increases reaction rate and selectivity while reducing byproduct content. Magnetic separation technology reduces waste residue, and bio-based plasticizers replace toxic solvents, meeting environmental standards.

[0043] It is important to note that the construction and arrangement of the present application, as illustrated in various exemplary embodiments, are illustrative only. Although only a few embodiments are described in detail in this disclosure, those reading this disclosure will readily appreciate that numerous modifications are possible (e.g., variations in the size, dimensions, structure, shape, and proportions of various components, as well as parameter values ​​(e.g., temperature, pressure, etc.), mounting arrangements, use of materials, color, orientation, etc.) without materially departing from the novel teachings and advantages of the subject matter described herein. For example, components shown as integrally formed may be constructed from multiple parts or components, the positions of components may be inverted or otherwise altered, and the nature, number, or position of discrete components may be modified or changed. All such modifications are therefore intended to be encompassed within the scope of this invention. The order or sequence of any process or method steps may be altered or resequenced according to alternative embodiments. In the claims, any "means-plus-function" clause is intended to cover structures described herein that perform the recited function, and not only structural equivalents but also equivalent structures. Other substitutions, modifications, changes, and omissions may be made in the design, operating conditions, and arrangement of the exemplary embodiments without departing from the scope of this invention. Therefore, the invention is not limited to the specific embodiments, but extends to various modifications that still fall within the scope of the appended claims.

[0044] Additionally, in order to provide a concise description of exemplary embodiments, all features of an actual embodiment may not be described (ie, those features that are not relevant to the best mode presently contemplated for carrying out the invention or those that are not relevant to implementing the invention).

[0045] It will be appreciated that in the development of any actual embodiment, as in any engineering or design project, numerous implementation-specific decisions may be made. Such a development effort may be complex and time-consuming, but will, for those of ordinary skill having the benefit of this disclosure, be a routine undertaking of design, fabrication, and production without undue experimentation.

[0046] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. A low freezing point production system for methyltriacetoxysilane, characterized in that: include, A pretreatment module (1) includes a premixing tank (11), wherein the premixing tank (11) is used for premixing raw materials; A reaction module (2) comprising a reaction tank (21) and a displacement member (22), wherein the displacement member (22) is disposed on the reaction tank (21) and is capable of communicating with an inner cavity of the reaction tank (21), the premixing tank (11) is connected to the displacement member (22) via a pipeline, and the premixed raw materials enter the reaction tank (21) via the displacement member (22); When a dynamic copolymerization reaction is carried out in the reaction tank (21), nitrogen is passed into the reaction tank (21) through the displacement member (22) to displace the air in the reaction tank (21).

2. The low freezing point production system of methyltriacetoxysilane according to claim 1, wherein: The replacement part (22) comprises a mounting shell (221) and an injection tube (222), wherein the injection tube (222) is used to inject liquid or gas into the reaction tank (21); The mounting shell (221) is arranged on the reaction tank (21), the injection tube (222) is inserted into the mounting shell (221), the injection tube (222) is elastically connected to the mounting shell (221), and the injection tube (222) can move in an axial direction relative to the mounting shell (221).

3. The low freezing point production system of methyltriacetoxysilane according to claim 2, characterized in that: A transition cavity (221a) is provided inside the mounting shell (221), and the contour shape of the end portion of the injection tube (222) located inside the mounting shell (221) can match the contour shape of the transition cavity (221a).

4. The low freezing point production system of methyltriacetoxysilane according to claim 3, characterized in that: The bottom of the mounting shell (221) is provided with a mounting hole (221b), the mounting hole (221b) is communicated with the transition cavity (221a), a first floating piece (223) is elastically installed in the mounting hole (221b), and the bottom of the mounting shell (221) is also provided with a first channel (221c), the first channel (221c) is communicated with the mounting hole (221b), and the first floating piece (223) switches the conduction or blocking state between the first channel (221c) and the transition cavity (221a) by floating itself.

5. The low freezing point production system of methyltriacetoxysilane according to claim 3 or 4, characterized in that: A second channel (221d) is further provided at the bottom of the installation shell (221), and the second channel (221d) is communicated with the transition cavity (221a); When the displacement member (22) is used to inject liquid into the reaction tank (21), the injection tube (222) is lifted by the liquid level and floats up until the second channel (221d) also flows with liquid; When the displacement member (22) is used to inject nitrogen into the reaction tank (21), the injection tube (222) is stationary relative to the mounting shell (221), and the second channel (221d) is used to discharge the displaced air in the reaction tank (21).

6. The low freezing point production system of methyltriacetoxysilane according to claim 3 or 4, characterized in that: A third channel (222a) is provided on the injection tube (222), and the third channel (222a) is used to connect the transition chamber (221a) and the outside of the reaction tank (21), and the displaced air in the reaction tank (21) is discharged through the second channel (221d) and the third channel (222a).

7. The low freezing point production system of methyltriacetoxysilane according to claim 6, characterized in that: A second floating sheet (224) is elastically installed in the third channel (222a), and the second floating sheet (224) is pushed by the displaced air to switch the conduction state between the transition chamber (221a) and the outside of the reaction tank (21).

8. The low freezing point production system of methyltriacetoxysilane according to claim 4, characterized in that: The first channel (221c) is arranged obliquely, and an extension line of the first channel (221c) intersects with the central axis of the installation shell (221).

9. A method for producing methyltriacetoxysilane at a low freezing point, characterized in that: include, Adding raw materials methyltrichlorosilane and ethyltriacetoxysilane into a premixing tank (11) for premixing; The raw materials are premixed and transferred to a reaction tank (21), where methyltrichlorosilane and ethyltriacetoxysilane are dynamically copolymerized under the action of a composite catalyst, during which nitrogen is passed through a displacement member (22) to replace air; Add sustained-release agents and control the release through ultrasound; Crystallization was inhibited synergistically by gradient cooling and ultrasound.

10. The method for producing methyltriacetoxysilane at a low freezing point according to claim 9, wherein: The composite catalyst is HMPA and nano-titanium dioxide-loaded phosphazene, with a mass ratio of 4:1; the cooling rate of the gradient cooling is controlled at 5°C / h in the 60-40°C stage and 1°C / h in the 40-20°C stage.

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