A method and equipment for preparing methylphenyl silicone oil

Abstract

The invention belongs to the field of silicone oil preparation, and specifically relates to a method for preparing methylphenyl silicone oil. The method comprises the following steps: adding a mixed solution of water, phenylchlorosilane and dimethyldichlorosilane into a preparation device, stirring and mixing the mixed solution uniformly in the preparation device, then dripping distilled water and an organic solvent mixed solution during the stirring process, standing the mixed solution to separate into upper and lower layers after the dripping is completed, separating an organic phase, washing the organic phase with alkaline water to neutrality, and then separating the layers again, adding a catalyst to the upper organic phase for reaction, washing the organic phase with water to neutrality after the reaction is completed, and then decompressing and distilling the mixed solution to obtain a methylphenyl silicone oil product; wherein the organic solvent is a mixture of two or more of distilled water, toluene, xylene, ether, chloroform and dichloromethane, including distilled water; the method can slowly add the original solution into the reactor under the action of a spiral feeding plate when the original solution is added into the reactor, and can also utilize the cooperation of the spiral feeding plate and a stirring component to stir the solution during the upper and lower circulation process, thereby improving the reaction efficiency.

Description

Technical Field

[0001] The invention belongs to the technical field of silicone oil preparation, and specifically relates to a method and equipment for preparing methylphenyl silicone oil. Background Art

[0002] The most common organic group in silicone oil is methyl, which is called methyl silicone oil, while methylphenyl silicone oil is the product in which part of the methyl group in methyl silicone oil is replaced by phenyl group. It has excellent high and low temperature resistance and lubricity, and has good development prospects.

[0003] Currently, there are many methods for preparing methylphenyl silicone oil. During the preparation process, it is usually necessary to manually add a mixed solution of distilled water and an organic solvent to allow the organic solvent to mix and react with the solution. However, it is difficult to control the rate and frequency of the manual addition of the mixed solution of distilled water and an organic solvent, which affects the preparation efficiency of the silicone oil, and therefore needs to be improved. Summary of the invention

[0004] The purpose of the present invention is to provide a method and equipment for preparing methylphenyl silicone oil, so as to solve the problems existing in the background technology.

[0005] In order to achieve the above technical objectives, the technical solution adopted by the present invention is as follows:

[0006] A method for preparing methylphenyl silicone oil comprises the following steps: adding a mixed solution of water, phenylchlorosilane and dimethyldichlorosilane into a preparation device, stirring and mixing the mixed solution uniformly in the preparation device, then dropping distilled water and an organic solvent mixed solution in the stirring process, standing the mixed solution to separate into upper and lower layers after the dropping is completed, separating an organic phase, washing it with alkaline water to neutrality, and then separating the layers again, adding a catalyst to the upper organic phase to react, washing it with water to neutrality after the reaction is completed, and then distilling the mixed solution under reduced pressure to obtain a methylphenyl silicone oil product;

[0007] The organic solvent is a mixture of two or more of toluene, xylene, ether, chloroform and dichloromethane;

[0008] The volume ratio of water, phenylchlorosilane and dimethyldichlorosilane is 5-15:1:1;

[0009] The volume ratio of the organic solvent to distilled water is 2-3:1.

[0010] A methylphenyl silicone oil preparation device comprises a reactor with a heating function, a feed pipe is rotatably installed at the center of the upper end of the reactor, a discharge pipe is installed at the lower end of the reactor, a fixed cylinder rotatably connected to the feed pipe is fixedly installed at the bottom of the reactor, a discharge port is provided at the lower part of the feed pipe, a feed port is provided at the lower part of the fixed cylinder, a spiral feed plate matching the fixed cylinder is fixedly installed on the feed pipe, a rotating shaft fixedly installed with the spiral feed plate is rotatably installed at the bottom of the reactor, a rotating cylinder matching the fixed cylinder is fixedly connected at the lower part of the feed pipe, a stirring assembly is fixedly installed on the circumference of the rotating cylinder, a dropping mechanism is fixedly installed on the upper end of the reactor, an exhaust assembly is installed on the reactor, a plurality of meshing teeth are fixedly installed on the circumference of the feed pipe, a driving gear meshing with the meshing teeth is rotatably connected to the upper end of the reactor, and a rotating motor transmission-connected to the driving gear is installed on the upper end of the reactor.

[0011] The dripping mechanism includes a driving component and several dripping components, several of the dripping components include a liquid storage cylinder fixedly installed on the reactor, a piston is sealingly and slidably connected inside the liquid storage cylinder, a connecting rod is installed on the upper end of the piston, a rectangular column is fixedly installed on the upper end of the connecting rod, a rotating joint is installed on the upper end of the rectangular column, and an annular water box is installed on the upper ends of several rotating joints. The connecting rod and the piston are provided with water inlet holes, and the water inlet holes are connected with the annular water box through the rotating joint. A one-way water inlet valve is installed inside the water inlet hole, a drip outlet is provided at the lower end of the liquid storage cylinder, a fine frustum matching the position of the drip outlet is installed at the lower end of the piston, and a sealing plug sealingly connected to the drip outlet is fixedly installed at the lower end of the fine frustum.

[0012] The driving assembly includes a driving motor, a threaded groove that is threadedly connected to the reactor is opened on the circumference of the connecting rod, the piston and the connecting rod are rotatably connected, the upper end of the driving motor is installed on the upper end of the reactor, the output end of the driving motor is installed with a first gear, the outer sides of several rectangular columns are sleeved with second gears, the upper end of the reactor is installed with a protective shell, several of the second gears and the first gear are meshed with an internal gear ring, and the protective shell is rotatably connected to the internal gear ring.

[0013] The stirring assembly comprises a plurality of stirring rods fixedly mounted on the rotating cylinder, and an arc-shaped plate matching the reaction kettle is mounted on the bottom of the rotating cylinder.

[0014] The spiral feeding plate and the rotating shaft are jointly fixedly mounted with a feeding table.

[0015] A liquid outlet box is installed between the discharge pipe and the reactor, a connecting port is provided between the liquid outlet box and the reactor, an inclined annular groove is provided inside the liquid outlet box, a circular ring is rotatably connected inside the liquid outlet box, a liquid blocking block sealingly connected to the connecting port is installed at the lower end of the circular ring, and a connecting component is installed between the circular ring and the reactor.

[0016] The present invention can add the original solution into the reactor slowly under the action of the spiral feeding plate, and can also use the cooperation of the spiral feeding plate and the stirring component to stir the solution during the up and down circulation, thereby improving the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention is further illustrated by means of the non-limiting examples given in the accompanying drawings.

[0018] Figure 1 This is a schematic structural diagram of a methylphenyl silicone oil preparation device of the present invention;

[0019] Figure 2 This is a schematic diagram of the first cross-sectional structure of a methylphenyl silicone oil preparation device of the present invention;

[0020] Figure 3 This is a second cross-sectional structural schematic diagram of a methylphenyl silicone oil preparation device of the present invention;

[0021] Figure 4 for Figure 3 A schematic diagram of the enlarged structure at A in the middle;

[0022] Figure 5 This is a third cross-sectional structural schematic diagram of a methylphenyl silicone oil preparation device of the present invention.

[0023] The main component symbols are described as follows:

[0024] Reactor 1, feed pipe 11, discharge pipe 12, fixed cylinder 13, spiral feed plate 14, rotating shaft 15, rotating cylinder 16, meshing teeth 17, driving gear 18, rotating motor 19, liquid storage cylinder 20, piston 21, connecting rod 22, rectangular column 23, rotary joint 24, annular water box 25, one-way water inlet valve 26, thin frustum 27, sealing plug 28, driving motor 30, first gear 31, second gear 32, protective shell 33, inner gear ring 34, stirring rod 40, arc plate 41, feed platform 42, liquid discharge box 43, connecting port 44, inclined annular groove 45, circular ring 46, liquid blocking block 47, connecting assembly 48. DETAILED DESCRIPTION

[0025] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0026] Example 1: Figure 1-5As shown, a methylphenyl silicone oil preparation device of the present invention comprises a reactor 1 with a heating function, a feed pipe 11 is rotatably installed at the center of the upper end of the reactor 1, a discharge pipe 12 is installed at the lower end of the reactor 1, a fixed cylinder 13 rotatably connected to the feed pipe 11 is fixedly installed at the bottom of the reactor 1, a discharge port is opened at the lower part of the feed pipe 11, a feed port is opened at the lower part of the fixed cylinder 13, a spiral feeding plate 14 matching the fixed cylinder 13 is fixedly installed at the feed pipe 11, and a spiral feeding plate 14 matching the fixed cylinder 13 is rotatably installed at the bottom of the reactor 1 The rotating shaft 15 is fixedly installed on the rotating feed plate 14, and the lower part of the feed pipe 11 is fixedly connected with a rotating cylinder 16 matching the fixed cylinder 13, and a stirring component is fixedly installed on the peripheral side of the rotating cylinder 16. A dropping mechanism is fixedly installed on the upper end of the reactor 1, and the reactor 1 is equipped with an exhaust component. A plurality of meshing teeth 17 are fixedly installed on the peripheral side of the feed pipe 11, and a driving gear 18 meshing with the meshing gear 17 is rotatably connected to the upper end of the reactor 1, and a rotating motor 19 transmission-connected to the driving gear 18 is installed on the upper end of the reactor 1.

[0027] When preparing silicone oil, the solution to be stirred for reaction is fed into the reactor 1 through the feed pipe 11. Since a spiral feed plate 14 is fixedly installed inside the feed pipe 11, the solution will flow into the reactor 1 along the upper plate surface of the spiral feed plate 14, thereby preventing the solution from being directly fed from top to bottom into the bottom of the reactor 1, thereby preventing the solution from causing large oscillations between the solutions and causing other reactions.

[0028] When the solution is added to the top of the discharge port, the rotating motor 19 is started to drive the driving gear 18 to rotate, and then the meshing teeth 17 and the feeding tube 11 are driven to rotate. The rotation of the feeding tube 11 will drive the spiral feeding plate 14 to rotate, so that the solution at the bottom moves upward with the cooperation of the fixed cylinder 13 and the spiral feeding plate 14, and then is discharged from the discharge port to the upper side of the solution. During the circulation of the solution, the rotating cylinder 16 will drive the stirring component to mix the solution on the surrounding side to improve the mixing efficiency. After the mixing is completed, the reagent is added by the dripping mechanism, so that the reagent is added to the solution of the reactor 1 in a dripping manner. Others generated during the reaction can be discharged from the exhaust component until the reaction is completed and the solution is allowed to stand and wait for stratification.

[0029] The solution inside is heated by the heating mechanism of the reactor 1 in the prior art, thereby adjusting the suitable reaction temperature of the solution.

[0030] The present invention can add the original solution into the reactor slowly under the action of the spiral feed plate 14, and can also use the spiral feed plate 14 and the stirring component to stir the solution during the up and down circulation process, thereby improving the reaction efficiency.

[0031] Embodiment 2: Further improvement is made on the basis of Embodiment 1, the dripping mechanism includes a driving component and a plurality of dripping components, the plurality of dripping components include a liquid storage cylinder 20 fixedly mounted on the reactor 1, a piston 21 is sealingly and slidably connected inside the liquid storage cylinder 20, a connecting rod 22 is mounted on the upper end of the piston 21, a rectangular column 23 is fixedly mounted on the upper end of the connecting rod 22, a rotary joint 24 is mounted on the upper end of the rectangular column 23, an annular water box 25 is mounted on the upper ends of the plurality of rotary joints 24, a water inlet hole is provided on the connecting rod 22 and the piston 21, the water inlet hole is connected to the annular water box 25 through the rotary joint 24, a one-way water inlet valve 26 is mounted inside the water inlet hole, a drip outlet is provided on the lower end of the liquid storage cylinder 20, a fine frustum 27 matching the position of the drip outlet is mounted on the lower end of the piston 21, a sealing plug 28 sealingly connected to the drip outlet is fixedly mounted on the lower end of the fine frustum 27.

[0032] In the initial state, the sealing plug 28 seals and blocks the drip port and the liquid storage cylinder 20 is located on the upper side of the liquid storage cylinder 20. At this time, the reagent solution to be added can be added through the water inlet at the upper end of the annular water box 25, and then the reagent passes through the rotary joint 24, the rectangular column 23, the connecting rod 22 and the one-way water inlet valve 26 to enter the liquid storage cylinder 20 for temporary storage. Then the driving component drives the annular water box 25 to move up and down, and the rectangular column 23, the connecting rod 22 and the piston 21 will be driven up and down during the up and down movement of the annular water box 25, and then the sealing plug 28 and the fine frustum 27 are driven downward during the downward movement of the piston 21. The diameter of the fine frustum 27 decreases from top to bottom, so when the fine frustum 27 is located at the drip port, a gap is formed with it, so that the solution inside the liquid storage cylinder 20 can slowly flow out from the gap and then drip into the solution inside the reactor 1. At the same time, if the dripping rate needs to be increased, the dripping rate of the dripping solution can be increased by driving the piston 21 to move downward to increase the pressure inside the liquid storage cylinder 20.

[0033] The driving assembly includes a driving motor 30, a thread groove threadedly connected to the reactor 1 is provided on the peripheral side of the connecting rod 22, the piston 21 and the connecting rod 22 are rotatably connected, the upper end of the driving motor 30 is installed on the upper end of the reactor 1, a first gear 31 is installed on the output end of the driving motor 30, a plurality of rectangular columns 23 are sleeved with second gears 32 on the outer sides, a protective shell 33 is installed on the upper end of the reactor 1, a plurality of second gears 32 and the first gear 31 are meshed with an inner gear ring 34, and the protective shell 33 is rotatably connected to the inner gear ring 34.

[0034] When the driving motor 30 is working, it will drive the first gear 31 to rotate. Since the first gear 31 is meshed with the inner gear ring 34, it will drive the inner gear ring 34 and the second gear 32 to rotate. Since the second gear 32 is sleeved on the outside of the rectangular column 23, the second gear 32 can slide up and down on the outside of the rectangular column 23, and when the second gear 32 rotates, it can drive the rectangular column 23 to rotate, so that the second gear 32 will drive the rectangular column 23 and the connecting rod 22 to rotate together. Since the threaded groove of the connecting rod 22 is threadedly connected to the reactor 1, when the connecting rod 22 rotates, the connecting rod 22 and the piston 21 will move, and then the piston 21 will be driven to move upward and downward through the forward and reverse rotation of the driving motor 30.

[0035] The stirring assembly includes a plurality of stirring rods 40 fixedly mounted on the rotating cylinder 16, and an arc plate 41 matching the reactor 1 is mounted at the bottom of the rotating cylinder 16; when the rotating cylinder 16 rotates, the stirring rods 40 will drive the plurality of stirring rods 40 to rotate to mix the solution, and the arc plate 41 matches the feeding direction of the spiral feeding plate 14. During the rotation of the rotating cylinder 16 and the spiral feeding plate 14, the arc plate 41 pushes the solution at the bottom toward the rotating cylinder 16, and then transports the solution near the periphery of the reactor 1 to the center, and then transports it upward for mixing.

[0036] The spiral feed plate 14 and the rotating shaft 15 are fixedly mounted with a feed table 42. The feed table 42 partially blocks the feed pipe 11, leaving only a gap at the head end of the spiral feed plate 14, thereby making it more convenient to contact the spiral feed plate 14 when feeding.

[0037] A liquid outlet box 43 is installed between the discharge pipe 12 and the reactor 1, a connecting port 44 is provided between the liquid outlet box 43 and the reactor 1, an inclined annular groove 45 is provided inside the liquid outlet box 43, a circular ring 46 is rotatably connected inside the liquid outlet box 43, a liquid blocking block 47 sealed with the connecting port 44 is installed at the lower end of the circular ring 46, and a connecting component 48 is installed between the circular ring 46 and the reactor 1.

[0038] During the operation of the reactor 1, the liquid blocking block 47 is connected to the sealing connection component 48 of the connecting port 44. When the stratification is completed and the lower layer liquid needs to be discharged, the connection of the connection component 48 is released, and then the ring 46 is driven to rotate, and then the liquid blocking block 47 leaks out of the connecting port 44, so that the solution flows from the connecting port 44 into the inclined annular groove 45, and is finally discharged from the discharge pipe 12. The flow to the surroundings through the connecting port 44 arranged on the peripheral side can avoid the upper solution from forming a circular vortex mixing the upper layer liquid and the lower layer liquid when the solution is discharged from the vertical direction, thereby affecting the stratification effect.

[0039] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the technology may modify or change the above embodiments without violating the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention.

Claims

1. A methylphenyl silicone oil preparation device, characterized in that: It comprises a reactor with a heating function, a feed pipe is rotatably installed at the center of the upper end of the reactor, a discharge pipe is installed at the lower end of the reactor, a fixed cylinder rotatably connected to the feed pipe is fixedly installed at the bottom of the reactor, a discharge port is opened at the lower part of the feed pipe, a feed port is opened at the lower part of the fixed cylinder, a spiral feeding plate matching the fixed cylinder is fixedly installed on the feed pipe, a rotating shaft fixedly installed with the spiral feeding plate is rotatably installed at the bottom of the reactor, a rotating cylinder matching the fixed cylinder is fixedly connected at the lower part of the feed pipe, a stirring assembly is fixedly installed on the circumference of the rotating cylinder, a dropping mechanism is fixedly installed on the upper end of the reactor, an exhaust assembly is installed on the reactor, a plurality of meshing teeth are fixedly installed on the circumference of the feed pipe, a driving gear meshing with the meshing teeth is rotatably connected to the upper end of the reactor, and a rotating motor transmission-connected to the driving gear is installed on the upper end of the reactor; The dripping mechanism includes a driving component and a plurality of dripping components, wherein the plurality of dripping components include a liquid storage cylinder fixedly mounted on the reactor, a piston is sealingly and slidably connected inside the liquid storage cylinder, a connecting rod is mounted on the upper end of the piston, a rectangular column is fixedly mounted on the upper end of the connecting rod, a rotating joint is mounted on the upper end of the rectangular column, an annular water box is mounted on the upper ends of the plurality of rotating joints, a water inlet hole is provided on the connecting rod and the piston, the water inlet hole is connected to the annular water box through a rotating joint, a one-way water inlet valve is mounted inside the water inlet hole, a dripping port is provided on the lower end of the liquid storage cylinder, a fine frustum matching the position of the dripping port is mounted on the lower end of the piston, and a sealing plug sealingly connected to the dripping port is fixedly mounted on the lower end of the fine frustum; The driving assembly includes a driving motor, a threaded groove that is threadedly connected to the reactor is opened on the circumference of the connecting rod, the piston and the connecting rod are rotatably connected, the upper end of the driving motor is installed on the upper end of the reactor, the output end of the driving motor is installed with a first gear, the outer sides of several rectangular columns are sleeved with second gears, the upper end of the reactor is installed with a protective shell, several of the second gears and the first gear are meshed with an internal gear ring, and the protective shell is rotatably connected to the internal gear ring.

2. A methylphenyl silicone oil preparation device according to claim 1, characterized in that: The stirring assembly comprises a plurality of stirring rods fixedly mounted on the rotating drum, and an arc-shaped plate matching the reaction kettle is mounted on the bottom of the rotating drum.

3. A methylphenyl silicone oil preparation device according to claim 1, characterized in that: The spiral feeding plate and the rotating shaft are jointly fixedly mounted with a feeding table.

4. A methylphenyl silicone oil preparation device according to claim 1, characterized in that: A liquid outlet box is installed between the discharge pipe and the reactor, a connecting port is provided between the liquid outlet box and the reactor, an inclined annular groove is provided inside the liquid outlet box, a circular ring is rotatably connected inside the liquid outlet box, a liquid blocking block sealingly connected to the connecting port is installed at the lower end of the circular ring, and a connecting component is installed between the circular ring and the reactor.

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