Methyl phenyl chlorosilane continuous hydrolysis device for preparing room temperature curing organic silicon resin coating

Abstract

The invention provides a methyl phenyl chlorosilane continuous hydrolysis device for preparing a room temperature curing organic silicon resin coating. The methyl phenyl chlorosilane continuous hydrolysis device comprises a methyl phenyl chlorosilane feeding pipeline, a water agent feeding pipeline and a reaction mixing chamber, a plurality of perforated plates are sequentially distributed in the reaction mixing chamber from front to back at intervals, a plurality of hydrolysis holes are uniformly distributed in the perforated plates at intervals, and a cooling jacket for cooling an inner cavity of the reaction mixing chamber is arranged on the outer wall of the reaction mixing chamber. The device is reasonable in structural design, and a methyl phenyl chlorosilane solution and water are secondarily dispersed to form a plurality of small flows when passing through the porous plate, so that the methyl phenyl chlorosilane solution and the water are fully mixed in the next-stage chamber. Meanwhile, a cooling jacket 7 is designed on the chamber wall of the reaction mixing chamber, heat generated in the reaction can be effectively exchanged, and the reaction temperature is kept stable, so that the stability of a product is ensured, and the hydrolysis quality is favorably improved.

Description

Technical Field

[0001] The invention relates to the technical field of hydrolysis equipment, and in particular to a methylphenylchlorosilane continuous hydrolysis device for preparing room temperature curing organic silicon resin coating. Background Art

[0002] Methylphenylchlorosilane is an organic compound and the main monomer for synthesizing silicone polymers. It is also an important component of room temperature curing silicone resin coatings. In the production of room temperature curing silicone resin coatings, the hydrolysis operation of methylphenylchlorosilane is usually carried out using a hydrolysis reactor. In the existing hydrolysis reactor, it is necessary to first add methylphenylchlorosilane solvent to the reactor, and then drip water into it for hydrolysis reaction. In this process, adding raw materials, hydrolysis, standing, and discharging all take a lot of time.

[0003] To this end, CN219003060U discloses a continuous hydrolysis device, including: a first material barrel for installing methylphenyl chlorosilane solvent, a first discharge pipe at its outlet, a first metering pump installed on the first discharge pipe; a second material barrel for installing water, a second discharge pipe at its outlet, a second metering pump installed on the second discharge pipe; a delivery pipe for conveying finished products; two atomizing nozzles are installed at the end of the delivery pipe, respectively connected to the first discharge pipe and the second discharge pipe; the atomizing nozzles are arranged relative to each other; at least two storage barrels, the inlet of which is connected in parallel with the delivery pipe, for storing hydrolyzed substances. The first metering pump inputs a fixed amount of methylphenyl chlorosilane solvent into the delivery pipe, and the second metering pump inputs a fixed amount of water into the delivery pipe; the methylphenyl chlorosilane solvent and water enter the delivery pipe for reaction, and are conveyed while reacting. When conveyed to the storage barrel, the finished product has been generated, and after static stratification, it is filled and transported, thereby improving production efficiency.

[0004] The above-mentioned continuous hydrolysis device is designed to make the hydrolysis reaction of methylphenylchlorosilane continuous by designing staggered partitions on the feed pipe to form an S-shaped flow channel, thereby extending the feed path, increasing turbulence, and promoting sufficient hydrolysis.

[0005] However, in practical applications, the hydrolysis reaction of methylphenylchlorosilane may be affected by conditions such as catalyst, temperature, pressure, etc., which may affect the reaction rate and the distribution of products, and good stirring and mixing effects can ensure that the reactants are fully contacted, thereby improving the reaction rate and the uniformity of the product. At the same time, the above-mentioned S-shaped flow channel only extends the reaction path, and the mixing between the methylphenylchlorosilane solution and water is only achieved by relative spraying of the atomizing nozzle. The solution mixed by the nozzle only relies on a little turbulence at the corner of the S-shaped flow channel for secondary mixing, and for the solution as a whole, it can not fully play the role of secondary stirring and mixing. Therefore, how to further control the temperature and pressure in the hydrolysis process in a continuous reaction, and fully mix the solution to improve the hydrolysis efficiency and hydrolysis quality has become a problem that needs to be solved at present. Summary of the invention

[0006] The technical problem to be solved by the present invention is: in order to overcome the shortcomings of the prior art, the present invention provides a methylphenylchlorosilane continuous hydrolysis device for preparing room temperature curing silicone resin coatings, which can perform continuous hydrolysis, control the temperature and pressure during the continuous hydrolysis process, and effectively control the reaction time of the mixture inside the hydrolysis device, so that the hydrolysis reaction is complete, the hydrolysis reaction rate is high and the product is stable.

[0007] The technical solution adopted by the present invention to solve the technical problem is: a methylphenylchlorosilane continuous hydrolysis device for preparing room temperature curing silicone resin coating, comprising a methylphenylchlorosilane feed pipeline, an aqueous agent feed pipeline, and a reaction mixing chamber; the front end of the reaction mixing chamber is connected to a feed pipe, and the rear end is connected to a discharge pipe; the discharge port of the methylphenylchlorosilane feed pipeline and the discharge port of the aqueous agent feed pipeline are respectively connected to the feed pipe pipeline of the reaction mixing chamber, and the discharge port of the methylphenylchlorosilane feed pipeline and the feed pipe pipeline of the reaction mixing chamber are respectively provided with metering pumps; a plurality of porous plates are sequentially spaced from front to back in the reaction mixing chamber, a plurality of hydrolysis holes are evenly spaced on the porous plates, and the diameter of the hydrolysis holes ranges from 1 mm to 2 mm, and the outer wall of the reaction mixing chamber is provided with a cooling jacket that cools the inner cavity of the reaction mixing chamber.

[0008] In the above scheme, methylphenylchlorosilane and water agent metering pumps are pumped into the reaction mixing chamber for mixing and reaction hydrolysis operations. In the reaction mixing chamber, the inner cavity of the reaction mixing chamber is divided into several chambers by a porous plate. When the mixed liquid passes through the porous plate, on the one hand, the mixing operation is completed, and on the other hand, the mixed liquid stays in the reaction mixing chamber for a certain time through the obstruction of the porous plate, thereby ensuring the hydrolysis time.

[0009] The mixing operation of the mixed liquid in the reaction mixing chamber includes:

[0010] 1. The mixed liquid in the previous chamber is diverted into the next chamber through the hydrolysis hole. During the process of passing through the hydrolysis hole, it is separated and then converged in the next chamber. The mixed liquid forms a process of confluence-diversion-convergence.

[0011] 2. When the mixed liquid flows in the reaction mixing chamber, it is blocked by the porous plate during the forward movement. A part of the mixed liquid enters the next chamber through the hydrolysis hole, and the other part of the mixed liquid impacts the porous plate with the flow of the liquid, forming turbulence at the plate without hydrolysis hole mesh, further achieving liquid mixing.

[0012] At the same time, heat is released during the hydrolysis of methylphenylchlorosilane, which causes the temperature to rise. In order to avoid the negative impact of the exothermic reaction on the hydrolysis process, heat exchange is performed through cooling water to maintain the temperature inside the reaction mixing chamber and keep it within the optimal reaction temperature range.

[0013] Furthermore, the hydrolysis holes on the porous plate are tapered holes, and the inner diameter of the tapered holes is a tapered structure that is larger at the front and smaller at the back along the flow direction of the solution in the reaction mixing chamber. The design of the tapered holes restricts the flow of the mixed liquid when it passes through the hydrolysis holes, and the flow rate increases through the reduced flow cross section, which facilitates the impact of the mixed liquid on the next porous plate, ensures the impact pressure of the liquid flow mixing in the reaction mixing chamber, effectively increases turbulence, improves the mixing effect, and thus improves the hydrolysis efficiency.

[0014] Preferably, the continuous hydrolysis device for preparing room temperature curing silicone resin coating with methylphenylchlorosilane also includes a storage barrel, and the end of the reaction mixing chamber is connected to a discharge port, and the discharge port is connected to the storage barrel through a pipeline. The storage barrel is used to receive the product after the hydrolysis in the reaction mixing chamber is completed, so as to effectively receive the product and store it for static storage during the continuous hydrolysis operation.

[0015] Preferably, the methylphenylchlorosilane feed pipeline includes a first raw material barrel, and the methylphenylchlorosilane to be hydrolyzed is installed in the first raw material discharge barrel; the first raw material barrel has a first discharge pipe at the bottom, and the first discharge pipe is connected to the feed pipe of the reaction mixing chamber through a first valve. The feeding of methylphenylchlorosilane can be effectively controlled by turning on and off the first valve, so that the feeding process can be accurately controlled.

[0016] Preferably, the aqueous solution feed pipeline includes a second raw material barrel, and the aqueous solution for hydrolysis reaction with methylphenylchlorosilane is installed in the second raw material discharge barrel; the second raw material barrel has a second discharge pipe at the bottom, and the second discharge pipe is connected to the feed pipe of the reaction mixing chamber after passing through the second valve. The feed of the aqueous solution can be effectively controlled by the on-off of the second valve, so that the feed process is accurately controllable and convenient for effectively adjusting the concentration of the solution in the hydrolysis.

[0017] Furthermore, the cooling jacket has a cooling water inlet at one end and a cooling water outlet at the other end, and both the cooling water inlet and the cooling water outlet are connected to an external cooling pump, and the cooling pump ensures the water temperature and circulation power of the cooling water.

[0018] Furthermore, the cooling water inlet is located on one side of the discharge pipe of the reaction mixing chamber, and the cooling water outlet is located on one side of the feed pipe of the reaction mixing chamber. That is, the overall flow direction of the cooling water is opposite to the overall flow direction of the mixed liquid in the reaction mixing chamber, so that in the tail end direction with the highest temperature, the cooling water with the lowest temperature performs efficient heat exchange to ensure the stability of the product.

[0019] The beneficial effect of the present invention is that the present invention provides a continuous hydrolysis device for methylphenyl chlorosilane for preparing room temperature curing silicone resin coating, which has a reasonable structural design. In the continuous hydrolysis device, the methylphenyl chlorosilane solution and water are secondary dispersed to form multiple small streams when passing through the porous plate, so as to be fully mixed in the next chamber. At the same time, the holes on the porous plate are further set, and the design of the conical holes enables the mixed solution to maintain the flow of the solution in the subsequent chamber through gradual contraction and pressurization when passing through the porous plate, and the reaction time of the mixture in the hydrolysis device is controllable, the hydrolysis rate is high, the product is stable, and the hydrolysis quality is high. A cooling jacket is designed on the wall of the reaction mixing chamber, and the heat generated in the reaction can be effectively heat exchanged to maintain the stability of the reaction temperature, thereby ensuring the stability of the product, which is conducive to improving the quality of hydrolysis. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0021] Figure 1 It is a structural diagram of embodiment 1 of the present invention.

[0022] Figure 2 It is a schematic diagram of the local flow direction at the position of the porous plate in the second embodiment of the present invention (the direction of the arrow is the flow direction).

[0023] Figure 3 Schematic diagram of the flow direction of the reaction mixing chamber and the cooling jacket in the third embodiment of the present invention (the direction of the arrow is the flow direction).

[0024] In the figure, 1, the first raw material barrel 2, the second raw material barrel 3, the first valve 4, the second valve 5, the metering pump 6, the reaction mixing chamber 7, the cooling jacket 8, the cooling water inlet 9, the cooling water outlet 10, the storage barrel 11, the porous plate 12, and the hydrolysis hole. DETAILED DESCRIPTION

[0025] The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic diagrams that only illustrate the basic structure of the present invention in a schematic manner, and therefore only show the components related to the present invention, and directions and references (e.g., up, down, left, right, etc.) may only be used to help describe the features in the drawings. Therefore, the following specific embodiments are not to be taken in a limiting sense, and the scope of the subject matter claimed is limited only by the attached claims and their equivalents.

[0026] Embodiment 1:

[0027] like Figure 1 The device for continuous hydrolysis of methylphenylchlorosilane for preparing room temperature curing silicone resin coating is the first embodiment of the present invention.

[0028] The continuous hydrolysis device comprises a methylphenylchlorosilane feed line, an aqueous solution feed line, a reaction mixing chamber 6 and a storage barrel 10. The reaction mixing chamber 6 is connected to a feed pipe at the front end and a discharge pipe at the rear end. A metering pump 5 is respectively arranged on the discharge port of the methylphenylchlorosilane feed line and the feed pipe pipeline of the reaction mixing chamber, and on the discharge port of the aqueous solution feed line and the feed pipe pipeline of the reaction mixing chamber. The inlet ends of the two metering pumps 5 are respectively connected to the discharge port of the methylphenylchlorosilane feed line and the discharge port pipeline of the aqueous solution feed line, and the outlet ends are connected to the feed port of the reaction mixing chamber 6. Metering pumps 5 are respectively arranged on the methylphenylchlorosilane feed line and the aqueous solution feed line, which can respectively accurately measure methylphenylchlorosilane and aqueous solution on the one hand, and can also avoid the two from being hydrolyzed in the front end pipe of the metering pump 5 on the other hand. Therefore, the shorter the pipeline between the outlet ends of the two metering pumps 5 and the feed port position of the reaction mixing chamber 6, the better.

[0029] The discharge port of the reaction mixing chamber 6 is connected to the storage barrel 10 through a pipeline. The storage barrel 10 is used to receive the product after the hydrolysis of the reaction mixing chamber 6 is completed, so as to effectively receive the product and store it for static storage during the continuous hydrolysis operation.

[0030] Specifically, the methylphenylchlorosilane feed line includes a first raw material barrel 1, and the methylphenylchlorosilane to be hydrolyzed is installed in the first raw material discharge barrel; the first raw material barrel 1 has a first discharge pipe at the bottom, and the first discharge pipe is connected to the feed pipe of the reaction mixing chamber 6 after passing through the first valve 3. The feeding of methylphenylchlorosilane can be effectively controlled by the on and off of the first valve 3, so that the feeding process can be accurately controlled.

[0031] The aqueous solution feeding pipeline includes a second raw material barrel 2, and the aqueous solution for hydrolysis reaction with methylphenylchlorosilane is installed in the second raw material discharge barrel; the second raw material barrel 2 has a second discharge pipe at the bottom, and the second discharge pipe is connected to the feed pipe of the reaction mixing chamber 6 after passing through the second valve 4. The feeding of the aqueous solution can be effectively controlled by the on-off of the second valve 4, so that the feeding process can be accurately controlled, which is convenient for effectively adjusting the concentration of the solution in the hydrolysis.

[0032] The valve may be, but is not limited to, a metering valve, a one-way solenoid valve, etc. The methylphenylsilyl chloride solution and the aqueous solution first pass through the valve and are pumped into the reaction mixing chamber 6 by the metering pump 5 for hydrolysis reaction. In this embodiment, the reaction mixing chamber 6 is mainly provided with two structures to influence and control the hydrolysis reaction.

[0033] 1. Several porous plates 11 are arranged in the reaction mixing chamber 6 at intervals along the direction of liquid flow. In Example 1, three porous plates 11 are arranged, and the three porous plates 11 divide the interior of the reaction mixing chamber 6 into four chambers arranged in sequence. After the methylphenylchlorosilane solution and the aqueous agent are pumped into the reaction mixing chamber 6 by the metering pump 5, they pass through the porous plates 11 in sequence and are discharged from the discharge pipe to the storage barrel 10. When the mixed liquid passes through the porous plates 11, it completes multiple mixing operations under the action of the porous plates 11. At the same time, due to the obstruction of the porous plates 11, the residence time of the mixed liquid in the reaction mixing chamber 6 is guaranteed to a certain extent, the hydrolysis time is guaranteed, and the material can be discharged after sufficient hydrolysis.

[0034] Specifically, the uniform mixing operation of the mixed liquid in the reaction mixing chamber 6 includes:

[0035] 1. The mixed solution in the previous chamber is divided into the next chamber through the hydrolysis hole 12. During the process of passing through the hydrolysis hole 12, it is separated and then converged in the next chamber. The mixed solution forms a process of confluence-division-confluence. The process of diversion and confluence is the process of secondary mixing of the mixed solution. In this embodiment, three diversion and confluence operations are realized through three porous plates 11. On the basis of the metering pump 5 pumping, three secondary mixing operations are continued in the hydrolysis process, which is more conducive to improving the efficiency of the hydrolysis reaction.

[0036] 2. When the mixed liquid flows in the reaction mixing chamber 6, the mixed liquid is blocked by the porous plate 11 during the movement from the previous chamber to the next chamber through the porous plate 11. In this process, a part of the mixed liquid enters the next chamber through the hydrolysis hole 12 for diversion and confluence. The other part of the mixed liquid collides with the liquid flow on the porous plate 11, forming turbulence at the plate without the mesh of the hydrolysis hole 12. The non-porous position of the porous plate 11 also realizes the mixing operation of the mixed liquid, further improving the mixing uniformity of methylphenylchlorosilane and water during the hydrolysis process.

[0037] Second, a cooling jacket 7 is designed on the outer wall of the reaction mixing chamber 6, and the temperature of the reaction mixing chamber 6 is controlled by circulating the coolant in the cooling jacket 7 to maintain the optimal temperature of the hydrolysis reaction.

[0038] Temperature has a significant effect on the hydrolysis reaction rate. Generally speaking, in the hydrolysis process, raising the temperature can accelerate the reaction rate, but too high a temperature may cause a side reaction, reduce product purity, and even cause a safety problem. Heat can be released during the hydrolysis of methylphenylchlorosilane, and this heat can cause the temperature to rise, in order to avoid the negative impact of the exothermic reaction on the hydrolysis process. Therefore, in the present embodiment, a cooling jacket 7 is designed, and heat exchange is carried out by cooling water, so that the reaction temperature can be accurately controlled, and the internal temperature of the reaction mixing chamber 6 is maintained, so that it is maintained within the range of the optimal reaction temperature, and it is avoided that too high or too low temperature has an adverse effect on the reaction.

[0039] The methylphenyl chlorosilane continuous hydrolysis device for preparing room temperature curing silicone resin coating designed in this way has a reasonable structural design. In the continuous hydrolysis device, the methylphenyl chlorosilane solution and water are secondary dispersed to form multiple small streams when passing through the porous plate 11, so as to be fully mixed in the next chamber. At the same time, a cooling jacket 7 is designed on the wall of the reaction mixing chamber 6, which can effectively exchange the heat generated in the reaction, keep the reaction temperature stable, thereby ensuring the stability of the product, which is conducive to improving the quality of hydrolysis.

[0040] Embodiment 2:

[0041] like Figure 2 The device for continuous hydrolysis of methylphenylchlorosilane for preparing room temperature curing silicone resin coating is the second embodiment of the present invention.

[0042] Embodiment 2 Based on Embodiment 1, the hole type and pore diameter of the hydrolysis hole 12 on the porous plate 11 are further set. Specifically, the hydrolysis hole 12 on the porous plate 11 is a conical hole, and the inner diameter of the conical hole is a tapered structure with a large front and a small back along the flow direction of the solution in the reaction mixing chamber 6. The minimum diameter of the small end of the conical hole is 1mm, and the maximum diameter of the large end of the conical hole is 2mm. The fine conical hole can more effectively divert the mixed solution into turbulence when the mixed solution passes through, so that the subsequent mixing is more uniform and effective.

[0043] The hole shape design of the conical hole restricts the flow of the mixed liquid when it passes through the hydrolysis hole 12. The flow velocity increases through the reduced flow cross-section. The gradual pressurization allows the solution to maintain flow and pressurized mixing in the subsequent cavity, making it easier for the mixed liquid to impact the next porous plate 11, ensuring the impact pressure of the liquid flow mixing in the reaction mixing chamber 6, effectively increasing turbulence, improving the mixing effect, and thus improving the hydrolysis efficiency.

[0044] Embodiment three:

[0045] like Figure 3 The device for continuous hydrolysis of methylphenylchlorosilane for preparing room temperature curing silicone resin coating is the third embodiment of the present invention.

[0046] Embodiment 3 Based on Embodiment 1, the cooling jacket 7 is further designed. The cooling jacket 7 has a cooling water inlet 8 at one end and a cooling water outlet 9 at the other end. The cooling water inlet 8 and the cooling water outlet 9 are both connected to an external cooling pump, and the cooling pump ensures the water temperature and circulation power of the cooling water. The cooling water inlet 8 is located on one side of the discharge pipe of the reaction mixing chamber 6, and the cooling water outlet is located on one side of the feed pipe of the reaction mixing chamber 6. That is, the overall flow direction of the cooling water is opposite to the overall flow direction of the mixed liquid in the reaction mixing chamber 6, so that in the direction of the highest temperature tail end, the cooling water with the lowest temperature performs efficient heat exchange, further ensuring the stability of the product.

[0047] Based on the above ideal embodiments of the present invention, the relevant staff can make various changes and modifications without departing from the technical concept of the present invention through the above description. The technical scope of the present invention is not limited to the contents of the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A continuous hydrolysis device for methylphenyl chlorosilane for preparing room temperature curing silicone resin coating, characterized in that: It includes a methylphenylchlorosilane feed pipeline, an aqueous agent feed pipeline, and a reaction mixing chamber (6); The reaction mixing chamber (6) has a front end connected to a feed pipe and a rear end connected to a discharge pipe; The discharge port of the methylphenylchlorosilane feed pipeline and the discharge port of the aqueous agent feed pipeline are respectively connected to the feed pipe of the reaction mixing chamber (6), and a metering pump (5) is respectively provided on the discharge port of the methylphenylchlorosilane feed pipeline and the feed pipe of the reaction mixing chamber, and on the discharge port of the aqueous agent feed pipeline and the feed pipe of the reaction mixing chamber; A plurality of porous plates (11) are sequentially spaced from front to back in the reaction mixing chamber (6), a plurality of hydrolysis holes (12) are evenly spaced on the porous plates (11), and the diameter of the hydrolysis holes ranges from 1 mm to 2 mm; The outer wall of the reaction mixing chamber (6) is provided with a cooling jacket (7) which is cooled with the inner cavity of the reaction mixing chamber (6).

2. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 1, characterized in that: The hydrolysis holes (12) on the porous plate (11) are tapered holes, and the inner diameter of the tapered holes is a tapered structure that is larger at the front and smaller at the back along the flow direction of the solution in the reaction mixing chamber (6).

3. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 1, characterized in that: It comprises a material storage barrel (10), and the end of the reaction mixing chamber (6) is provided with a discharge port, and the discharge port is connected to the material storage barrel (10) through a pipeline.

4. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 1, characterized in that: The methylphenylchlorosilane feed pipeline comprises a first raw material barrel (1), and the methylphenylchlorosilane to be hydrolyzed is installed in the first raw material discharge barrel; the first raw material barrel (1) has a first discharge pipe at the bottom, and the first discharge pipe is connected to the feed pipe of the reaction mixing chamber (6) after passing through a first valve (3).

5. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 1, characterized in that: The aqueous agent feeding pipeline comprises a second raw material barrel (2), and the aqueous agent for hydrolyzing with methylphenylchlorosilane is installed in the second raw material discharge barrel; the second raw material barrel (2) has a second discharge pipe at the bottom, and the second discharge pipe is connected to the feed pipe of the reaction mixing chamber (6) after passing through a second valve (4).

6. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 1, characterized in that: The cooling jacket (7) has a cooling water inlet (8) at one end and a cooling water outlet (9) at the other end. The cooling water inlet (8) and the cooling water outlet (9) are both connected to an external cooling pump.

7. The continuous hydrolysis device for preparing room temperature curing silicone resin coating according to claim 6, characterized in that: The cooling water inlet (8) is located on one side of the discharge pipe of the reaction mixing chamber (6), and the cooling water outlet is located on one side of the feed pipe of the reaction mixing chamber (6).

Images