Process and apparatus for preparing aqueous fluorosilicone resins

Abstract

The application relates to the field of water-based fluorosilicone resin preparation, in particular to a water-based fluorosilicone resin preparation method and device, which comprises a tank body, the inside of the tank body is provided with a hollow stirring piece, the top of the tank body is provided with a feeding cylinder, the feeding cylinder is fixedly connected with the stirring piece, the inside of the stirring piece is provided with a pressing sheet and a base sheet which are distributed upwards and downwards, a rubber tube is sealed between the pressing sheet and the base sheet, the pressing sheet and the base sheet are vertically and elastically connected through a spring, a slide is arranged on the inner wall of the tank body, the slide has a height difference around the tank body, a slide handle is slidably arranged in the slide, a vertical and extending lifting groove is arranged on the surface of the stirring piece, and the slide handle penetrates through the lifting groove and is fixedly connected with the pressing sheet. During the stirring process of the stirring piece on the polymerization material, the pressing sheet and the base sheet are intermittently closed to automatically and intermittently introduce an initiator into the tank body, the initiator is uniformly added, the polymerization of the water-based fluorosilicone resin is stably carried out, and the water-based fluorosilicone resin can be simultaneously and massively produced.

Description

Technical Field

[0001] This invention relates to the field of waterborne fluorosilicone resin preparation, and more particularly to a method and apparatus for preparing waterborne fluorosilicone resin. Background Technology

[0002] The preparation of waterborne fluorosilicone resins often involves mixing fluorinated acid ester monomers and silane monomers in an organic solvent to form a homogeneous system, then adding an initiator and mixing to carry out a polymerization reaction, thereby obtaining a waterborne fluorosilicone resin copolymer.

[0003] The addition of the initiator is particularly important in the entire polymerization reaction. It needs to be added slowly during the mixing process. In the traditional preparation process, the initiator is added dropwise. When the amount of waterborne fluorosilicone resin prepared at one time is large, the work intensity of uniformly adding the initiator is high, and it is difficult for the existing equipment to maintain uniform addition of the initiator. Summary of the Invention

[0004] The purpose of this invention is to solve the following problems existing in the prior art: In the traditional preparation process, the initiator is added by dripping. When the amount of waterborne fluorosilicone resin prepared at one time is large, the work intensity of uniformly adding the initiator is high, and it is difficult for existing equipment to maintain uniform addition of the initiator.

[0005] To address the problems existing in the prior art, this invention provides an apparatus for preparing water-based fluorosilicone resin, comprising a tank body, a hollow stirring element inside the tank body, a feeding cylinder at the top of the tank body, the feeding cylinder being fixedly connected to the stirring element, a pressing plate and a substrate plate arranged vertically inside the stirring element, a rubber tube sealing between the pressing plate and the substrate plate, and the pressing plate and the substrate plate being vertically elastically connected by a spring, a slide rail being formed on the inner wall of the tank body, the slide rail extending around the tank body with a height difference, a sliding handle sliding within the slide rail, a vertically extending lifting groove being formed on the surface of the stirring element, the sliding handle passing through the lifting groove and being fixedly connected to the pressing plate, the upper part of the rubber tube being connected to the feeding cylinder through a first one-way valve, and the lower part of the rubber tube being connected to the inside of the tank body through a second one-way valve.

[0006] Preferably, the stirring component includes a shaft cylinder, a shaft tube extending through the bottom of the shaft cylinder, multiple handle tubes evenly extending through the bottom of the shaft tube, the ends of the handle tubes extending through the interior of the tank, a feeding cylinder fixedly connected to the top of the shaft cylinder, a motor being connected to the feeding cylinder via a transmission belt, and a second one-way valve extending through the interior of the shaft tube.

[0007] Preferably, the substrate and the pressing plate are adapted to slide within the shaft tube, and the substrate and the pressing plate are vertically aligned and slidably guided by a guide groove and a guide post. A heater is provided inside the tank at the upper part of the shaft tube, and the upper part of the shaft tube is connected to the heater through a third one-way valve. A fourth one-way valve is provided at the bottom of the shaft tube.

[0008] Preferably, the heater includes two panels distributed vertically, with a spiral channel between the two panels. The outer part of the spiral channel has an air inlet that penetrates the lower part of the inner cavity of the tank. The third one-way valve is disposed inside the spiral channel, and an opening for aligning the third one-way valve is provided on the surface of the shaft tube. An electric heating element is disposed inside the spiral channel.

[0009] Preferably, the substrate has a feed tube at the bottom, the feed tube passes through the rubber tube, the diameter of the feed tube is smaller than the inner diameter of the shaft tube, and the bottom of the feed tube is lower than the opening.

[0010] Preferably, the height difference of the slide is greater than the movable height of the substrate within the shaft cylinder.

[0011] Preferably, the handle tube is connected to the bottom of the shaft tube, the handle tube extends downward at an angle, the bottom end of the handle tube is bent to a horizontal shape, and both the bottom end of the handle tube and the horizontally bent part have an opening that penetrates the inner cavity of the tank.

[0012] A method for preparing an aqueous fluorosilicone resin based on the aforementioned aqueous fluorosilicone resin preparation apparatus comprises the following steps:

[0013] A. Fluorine-containing acid ester monomers and silane-containing monomers are quantitatively placed in an organic solvent inside a tank, and the stirring element is rotated by a motor to form a homogeneous system inside the tank.

[0014] B. Place the diluted initiator in the feeding cylinder. During the rotation of the agitator, the slide handle slides along the slide rail, causing the slide handle to drive the press to move up and down continuously. When the press rises, the press moves away from the substrate and the rubber tube expands under the action of elasticity. The initiator in the feeding cylinder is drawn into the rubber tube through the first one-way valve. When the press falls, the press moves closer to the substrate and compresses the rubber tube. The initiator in the rubber tube is sprayed into the tank through the second one-way valve.

[0015] C. While the agitator is continuously stirring, the initiator is continuously and evenly sprayed into the tank.

[0016] Compared with related technologies, the waterborne fluorosilicone resin preparation method and apparatus provided by the present invention have the following beneficial effects:

[0017] In this invention, during the stirring of the polymer material by the agitator, the tablet and substrate are intermittently closed to automatically introduce the initiator into the tank intermittently, keeping the initiator added evenly, so that the polymerization of waterborne fluorosilicone resin can proceed stably, and it is convenient to produce waterborne fluorosilicone resin in large quantities at the same time.

[0018] In this invention, when stirring polymer materials, circulating nitrogen gas inside the tank is introduced into the material through the movement of the substrate piston, which is beneficial for rapid mixing of the material and for uniform discharge of the initiator assisted by nitrogen gas.

[0019] The present invention incorporates a heater inside the tank to heat circulating nitrogen gas and uses hot bubbles to heat the mixture, thereby maintaining a stable polymerization reaction temperature. Attached Figure Description

[0020] Figure 1 This is one of the overall structural schematic diagrams of the present invention;

[0021] Figure 2 This is the second schematic diagram of the overall structure of the present invention;

[0022] Figure 3 This is a schematic diagram of the internal structure of the tank of the present invention;

[0023] Figure 4 This is a schematic diagram of the stirring component structure of the present invention;

[0024] Figure 5 This is a schematic diagram of the substrate and pressing structure of the present invention;

[0025] Figure 6 This is a schematic diagram of the heater structure of the present invention.

[0026] Numbered in the diagram: 1. Tank body; 11. Inlet; 12. Outlet; 2. Feeding cylinder; 3. Motor; 4. Heater; 41. Panel; 42. Spiral channel; 43. Air inlet; 44. Heating element; 5. Shaft tube; 51. Handle tube; 52. Port; 53. Third check valve; 54. Fourth check valve; 6. Shaft tube; 61. Base plate; 62. Pressing plate; 63. Rubber tube; 64. Feed pipe; 65. First check valve; 66. Second check valve; 67. Guide groove; 68. Guide column; 7. Slide rail; 8. Slide handle; 81. Lifting groove. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0028] The specific implementation of the present invention will be described in detail below with reference to specific embodiments. Example 1

[0029] like Figure 1-2 As shown, an apparatus for preparing waterborne fluorosilicone resin includes a tank 1, an inlet 11 on the side of the tank 1, and a outlet 12 at the bottom of the tank 1.

[0030] like Figure 3-4As shown, the stirring component includes a shaft cylinder 6, with a shaft tube 5 concentrically fixed at the bottom of the shaft cylinder 6. The diameter of the shaft tube 5 is smaller than the diameter of the shaft cylinder 6. The shaft tube 5 and the shaft cylinder 6 are distributed along the axis of the tank body 1 inside the tank body 1. A feeding cylinder 2 with an open top is provided at the top of the tank body 1. The bottom of the feeding cylinder 2 rotates through the top of the tank body 1 and is fixedly connected to the shaft cylinder 6. Multiple handles 51 are evenly distributed at the bottom end of the shaft tube 5. The handles 51 are connected to the bottom of the shaft tube 5, and the handles 51 extend downward at an angle close to the bottom of the tank body 1. The bottom end of the handles 51 is bent to a horizontal position. The bottom end of the handles 51 and the horizontally bent part both have an opening that penetrates the inner cavity of the tank body 1.

[0031] The motor 3 is installed on the surface of the tank 1, and the shaft end of the motor 3 is connected to the feeding cylinder 2 via belt drive.

[0032] like Figure 5 As shown, pressure plates 62 and base plates 61 are distributed vertically inside the shaft cylinder 6. The position of the base plate 61 is positioned, and a guide post 68 is fixed on the upper surface of the base plate 61. A guide groove 67 is opened on the bottom surface of the pressure plate 62. The pressure plate 62 and the base plate 61 maintain vertical telescopic sliding through the guide groove 67 and the guide post 68, which are connected in a straight line. A rubber tube 63 is sealed between the pressure plate 62 and the base plate 61. A spring is sleeved on the outside of the rubber tube 63 to make the pressure plate 62 and the base plate 61 vertically elastically connected. A vertically extending lifting groove 81 is opened on the edge of the shaft cylinder 6. A sliding handle 8 is passed through the lifting groove 81 and fixedly connected to the side of the pressure plate 62. A slide 7 is opened around the inner wall of the tank body 1. The slide 7 extends around the tank body 1 with a height difference. A roller is rotatably installed at the end of the sliding handle 8. The roller is adapted to the slide 7.

[0033] A first check valve 65 is provided at the bottom of the feeding cylinder 2, which extends downward through the shaft cylinder 6. The top of the rubber tube 63 is connected to the first check valve 65 through a flexible hose. A second check valve 66 is provided at the bottom of the rubber tube 63, which extends downward through the shaft cylinder 5.

[0034] Organic solvents, fluorinated acid ester monomers, and silane monomers are placed inside tank 1 through inlet 11. Diluted initiator is placed in feeding cylinder 2, and inlet 11 is sealed. Nitrogen gas is filled into tank 1. Motor 3 is turned on to drive feeding cylinder 2, shaft cylinder 6, shaft tube 5, and handle tube 51 to rotate. The evenly distributed handle tube 51 stirs the materials in tank 1 to form a homogeneous system. At the same time, as the sliding handle 8 rotates with the shaft cylinder 6, the sliding handle 8 is guided by the slide rail 7 to cause the tablet 62 to move up and down intermittently. When the tablet is pressed... When the tablet 62 rises away from the substrate 61, the rubber tube 63 unfolds under the action of elasticity, and a negative pressure is generated inside the rubber tube 63. The initiator in the feed cylinder 2 is drawn into the rubber tube 63 through the first one-way valve 65. When the tablet 62 approaches the substrate 61, the rubber tube 63 is compressed. The initiator in the rubber tube 63 is sprayed into the shaft tube 5 through the second one-way valve 66, and then introduced into the mixing system through the handle tube 51. The continuous rotation and stirring realizes the continuous and uniform introduction of the initiator into the mixing system, so that the polymerization reaction proceeds in an orderly manner. Example 2

[0035] like Figure 4-5 As shown, the tablet 62 and the substrate 61 are adapted to slide inside the shaft cylinder 6. A rubber ring is provided on the edge of the substrate 61 so that the substrate 61 can make a lifting piston movement inside the shaft cylinder 6. The height difference of the slide 7 is greater than the height of the substrate 61 in the shaft cylinder 6. A feed pipe 64 is fixedly connected to the bottom of the substrate 61. The diameter of the feed pipe 64 is smaller than the inner diameter of the shaft tube 5. A second one-way valve 66 is provided inside the feed pipe 64. A port 52 is opened at the upper part of the shaft tube 5. The port 52 is connected to the upper end of the tank body 1 through a third one-way valve 53. A fourth one-way valve 54 is provided at the lower part of the shaft tube 5.

[0036] When the feeding cylinder 2, shaft cylinder 6, shaft tube 5, and handle tube 51 rotate, the pressing plate 62 and the substrate 61 are driven by the sliding handle 8 to maintain continuous lifting and lowering movement. The gap between the bottom of the substrate 61 and the shaft cylinder 6 forms an air cavity. When the substrate 61 rises, the air cavity expands, and nitrogen gas from the upper part of the tank 1 is drawn into the air cavity through the third one-way valve 53. When the substrate 61 falls, the air cavity is compressed, and nitrogen gas is introduced into the handle tube 51 through the fourth one-way valve 54 and then evenly sprayed into the bottom of the tank 1 to form several bubbles, which accelerates the mixing of materials.

[0037] After the substrate 61 slides into contact with the bottom of the shaft cylinder 6, the continuously pressing plate 62 will cause the rubber tube 63 to compress the initiator.

[0038] The nitrogen gas that conducts the initiator helps to conduct the initiator, which is beneficial for the initiator to mix quickly in the material. Example 3

[0039] like Figure 4-6As shown, the heater 4 is located at the lower part of the shaft tube 6. The heater 4 includes two panels 41 distributed vertically. The shaft tube 5 rotates through the two panels 41. The port 52 is located between the two panels 41. A spiral channel 42 is provided between the two panels 41. An electric heating element 44 is provided in the spiral channel 42. The outer part of the spiral channel 42 has an air inlet 43 that penetrates the lower part of the inner cavity of the tank body 1. A third one-way valve 53 is provided inside the spiral channel 42.

[0040] During the mixing process, the heating element 44 is turned on to generate heat, and the air in the spiral channel 42 is heated. The nitrogen in the upper part of the tank 1 enters the spiral channel 42 through the air inlet 43 and is heated. The heated nitrogen enters the shaft tube 5 through the third one-way valve 53 and the port 52 and is evenly introduced downward into the mixture. The high-temperature bubbles formed heat the polymer material and keep the polymerization reaction at about 70°C. Example 4

[0041] A method for preparing an aqueous fluorosilicone resin based on the aforementioned aqueous fluorosilicone resin preparation apparatus comprises the following steps:

[0042] A. Fluorine-containing acid ester monomers and silane-containing monomers are quantitatively placed in the organic solvent in tank 1, and the stirring element is rotated by motor 3 to form a homogeneous system in tank 1.

[0043] B. Place the diluted initiator in the feeding cylinder 2. During the rotation of the agitator, slide the handle 8 along the slide rail 7, causing the handle 8 to drive the pressing plate 62 to move up and down continuously. When the pressing plate 62 rises, the pressing plate 62 moves away from the base plate 61 and the rubber tube 63 expands under the action of elasticity. The initiator in the feeding cylinder 2 is drawn into the rubber tube 63 through the first one-way valve 65. When the pressing plate 62 falls, the pressing plate 62 moves closer to the base plate 61 and compresses the rubber tube 63. The initiator in the rubber tube 63 is sprayed into the tank 1 through the second one-way valve 66.

[0044] C. While the agitator is continuously stirring, the initiator is continuously and evenly sprayed into the tank 1.

Claims

1. An apparatus for preparing water-based fluorosilicone resin, comprising a tank (1), characterized in that, The tank (1) has a hollow stirring component inside. The top of the tank (1) has a feeding cylinder (2) which is fixedly connected to the stirring component. The stirring component has a pressure plate (62) and a base plate (61) distributed vertically inside. A rubber tube (63) is sealed between the pressure plate (62) and the base plate (61). The pressure plate (62) and the base plate (61) are vertically elastically connected by a spring. The inner wall of the tank (1) has a slide (7) which extends around the tank (1) with a height difference. A sliding handle (8) slides inside the slide (7). A vertically extending lifting groove (81) is opened on the surface of the stirring component. The sliding handle (8) passes through the lifting groove (81) and is fixedly connected to the pressure plate (62). The upper part of the rubber tube (63) is connected to the feeding cylinder (2) through a first one-way valve (65), and the lower part of the rubber tube (63) is connected to the inside of the tank (1) through a second one-way valve (66). The stirring component includes a shaft cylinder (6), a shaft tube (5) passing through the bottom of the shaft cylinder (6), a plurality of handle tubes (51) passing through the bottom of the shaft tube (5), the ends of the handle tubes (51) passing through the inside of the tank body (1), a feeding cylinder (2) being fixedly connected to the top of the shaft cylinder (6), a motor (3) being connected to the feeding cylinder (2) via a transmission belt, and a second one-way valve (66) passing through the inside of the shaft tube (5). The substrate (61) and the pressing plate (62) are adapted to slide inside the shaft cylinder (6). The substrate (61) and the pressing plate (62) are vertically inserted and slidably guided by the vertically aligned guide groove (67) and guide post (68). The tank body (1) is equipped with a heater (4) located at the upper part of the shaft tube (5). The upper part of the shaft tube (5) is connected to the heater (4) through the third one-way valve (53). The bottom of the shaft tube (5) is equipped with a fourth one-way valve (54).

2. The apparatus for preparing waterborne fluorosilicone resin according to claim 1, characterized in that, The heater (4) includes two panels (41) distributed vertically, with a spiral channel (42) between the two panels (41). The outer part of the spiral channel (42) has an air inlet (43) that penetrates the lower part of the inner cavity of the tank (1). The third one-way valve (53) is located inside the spiral channel (42). The surface of the shaft tube (5) is provided with a port (52) for aligning the third one-way valve (53). The spiral channel (42) is provided with an electric heating element (44).

3. The apparatus for preparing waterborne fluorosilicone resin according to claim 2, characterized in that, The substrate (61) has a feed tube (64) at the bottom, which passes through the rubber tube (63). The diameter of the feed tube (64) is smaller than the inner diameter of the shaft tube (5), and the bottom of the feed tube (64) is lower than the position of the opening (52).

4. The apparatus for preparing waterborne fluorosilicone resin according to claim 1, characterized in that, The height difference of the slide (7) is greater than the height of the substrate (61) within the cylinder (6).

5. The apparatus for preparing waterborne fluorosilicone resin according to claim 1, characterized in that, The handle (51) is connected to the bottom of the shaft tube (5). The handle (51) extends downward at an angle. The bottom end of the handle (51) is bent to a horizontal position. The bottom end of the handle (51) and the horizontally bent part both have an opening that penetrates the inner cavity of the tank body (1).

6. A method for preparing an aqueous fluorosilicone resin based on the apparatus for preparing an aqueous fluorosilicone resin according to any one of claims 1-5, characterized in that, The specific steps are as follows: A. Fluorine-containing acid ester monomers and silane-containing monomers are quantitatively placed in the organic solvent inside the tank (1), and the stirring element is rotated by the motor (3) to form a uniform system inside the tank (1); B. Place the diluted initiator in the feeding cylinder (2). During the rotation of the stirring component, slide handle (8) slides along slide rail (7) to drive the pressing plate (62) to move up and down continuously. When the pressing plate (62) rises, the pressing plate (62) moves away from the substrate (61) and the rubber tube (63) expands under the action of elasticity. The initiator in the feeding cylinder (2) is sucked into the rubber tube (63) through the first one-way valve (65). When the pressing plate (62) falls, the pressing plate (62) moves close to the substrate (61) and compresses the rubber tube (63). The initiator in the rubber tube (63) is sprayed into the tank (1) through the second one-way valve (66). C. While the agitator is continuously stirring, the initiator is continuously and evenly sprayed into the tank (1).

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