LCD microsphere preparation device and preparation method thereof

Abstract

The present invention relates to the field of microsphere technology, and in particular to a device for preparing LCD microspheres and a method for preparing the same. Provided is a device for preparing LCD microspheres and a method for preparing the same. A device for preparing LCD microspheres and a method for preparing the same, comprising a bottom plate, a liquid storage glass bottle, a funnel, an electric push rod, a vacuum drying oven, a transparent insulation box, and a reaction bottle, etc.; a liquid storage glass bottle is placed on the bottom plate, the bottle mouth of the liquid storage glass bottle is fixedly connected to the funnel, electric push rods are evenly distributed and installed on the bottom plate, the movable rod of the electric push rod is fixedly connected to the funnel, a vacuum drying oven is installed on one side of the bottom plate, a transparent insulation box is fixedly connected to the bottom plate through a vertical rod, and a reaction bottle is placed in the transparent insulation box. A high-pressure mercury lamp is used in combination with an ultraviolet light initiator to achieve rapid polymerization of polymerizable monomers. Due to the gradient decrease in the intensity of ultraviolet light transmission, the polymerizable monomers will show the characteristics of polymerization speed with the intensity of the ultraviolet light, and a microsphere liquid crystal with a core-shell structure can be quickly obtained during the stirring process.

Description

Technical Field

[0001] The present invention relates to the technical field of microspheres, and in particular to a device and method for preparing LCD microspheres. Background Art

[0002] Microspheres are the basic materials of modern industry. With the development of liquid crystal technology, microspheres are widely used as spacer materials for liquid crystal displays. For LCD displays, as today's displays become larger and larger, it is increasingly difficult to maintain a fixed spacing between two glass plates. For large screens, the uneven thickness of the glass plates leads to uneven thickness of the liquid crystal layer between the glass plates, making it difficult to maintain consistent display clarity.

[0003] Microspheres are used to fill the space between the glass plates to keep the glass plates parallel. At this moment, the microspheres are like the skeleton of the glass plates, supporting the gap space between the two glass plates. In addition, the liquid crystal itself is fluid, and it needs to be encapsulated during the application process, which brings limitations to the application. If the liquid crystal is encapsulated in a solid shell and made into a spherical shape and injected between the glass plates, it can provide support like spacer microspheres, and can also reduce the addition of polymer microspheres to improve screen clarity. Summary of the invention

[0004] In order to overcome the disadvantage that liquid crystal has certain limitations in its fluidity during application, a device and method for preparing LCD microspheres are provided.

[0005] Technical solution: A device for preparing LCD microspheres, including a base plate, a liquid storage glass bottle, a funnel, an electric push rod, a vacuum drying oven, a transparent insulation box, a reaction bottle and a high-pressure mercury lamp. The liquid storage glass bottle is placed on the base plate, the mouth of the liquid storage glass bottle is fixedly connected to the funnel, the electric push rods are evenly distributed on the base plate, the movable rods of the electric push rods are fixedly connected to the funnel, the vacuum drying oven is installed on one side of the base plate, the transparent insulation box is fixedly connected to the base plate through a vertical rod, the reaction bottle is placed in the transparent insulation box, and the high-pressure mercury lamp is installed on the side of the transparent insulation box close to the reaction bottle.

[0006] In a preferred embodiment of the present invention, a heating jacket is also included, and the heating jacket is installed at the bottom of the reaction bottle.

[0007] In a preferred embodiment of the present invention, it also includes a motor, an agitator and a bottle cap. The bottle cap is screwed on the top of the reaction bottle, the motor is installed on the bottle cap, and the output shaft of the motor is connected to the agitator.

[0008] In a preferred embodiment of the present invention, an annular cover plug is further included, and a feeding port is opened on the bottle cap, and the feeding port is closed by the annular cover plug.

[0009] In a preferred embodiment of the present invention, a glass stopper rod is further included. A round hole is opened at the bottom of the reaction bottle. The round hole protrudes and passes through the bottom of the transparent insulation box. The glass stopper rod is slidably placed in the round hole. The glass stopper rod falls due to gravity to keep the round hole closed.

[0010] In a preferred embodiment of the present invention, it also includes an L-shaped guide frame, a partition and a filter frame. A notch is opened on the vacuum drying box, and the two sides of the notch are fixedly connected to the L-shaped guide frames opposite to each other. The filter frame is slidably connected to the L-shaped guide frame, and the partition is slidably connected to the notch. The filter frame can be airtightly attached to the bottom of the transparent insulation box as the funnel moves upward, and the glass stopper rod is lifted.

[0011] In a preferred embodiment of the present invention, an annular plug is further included. The annular plug is fixedly connected to the bottom of the transparent heat preservation box to surround the glass plug rod that passes through. A circular groove is opened on the filter frame, and the circular groove and the annular plug are in airtight fit.

[0012] In a preferred embodiment of the present invention, it also includes a liquid storage box, a conduit and a filter head. The vacuum drying box and the transparent insulation box are fixedly connected to the liquid storage box. The bottom of the liquid storage box is connected to the conduit. The filter head is arranged at the bottom of the conduit, and the filter head is arranged above the L-shaped guide frame.

[0013] In a preferred embodiment of the present invention, the preparation method of LCD microspheres comprises the following steps: 1) adding water, hydroxyethyl cellulose, tricalcium phosphate and polyvinyl pyrrolidone in a ratio of 50000:39:10:3 into a reaction bottle, wherein polyvinyl pyrrolidone is used as a dispersing and suspending medium, and simultaneously adding 0.5-0.55 times the mass of water pentaerythritol tetraacrylate and 1.2-1.3 times the mass of water liquid crystal, wherein the pentaerythritol tetraacrylate contains 25% 1,6-hexanediol acrylate, 4.3% ultraviolet absorber, 3.6% ultraviolet photoinitiator and 0.3% tert-butyl peroxybenzoate;

[0014] 2) Turn on the high-pressure mercury lamp to irradiate the reaction bottle;

[0015] 3) Cover the bottle cap and place the stirrer in the reaction bottle, control the temperature of the heating jacket between 90-110 degrees Celsius and start stirring with the stirrer;

[0016] 4) After the reaction is completed, filter paper is placed on the filter frame, and the electric push rod is started to move the funnel and the liquid storage glass bottle upward. The funnel fits the bottom of the filter frame, and the annular plug is inserted into the circular groove on the filter frame. After the funnel, the filter frame and the annular cover plug are in close contact, the filter frame lifts the glass plug rod, and the mixed liquid in the reaction bottle flows into the filter frame. The air extraction interface of the liquid storage glass bottle is connected to the vacuum pump, and the annular cover plug is opened. The vacuum pump extracts air from the liquid storage glass bottle to form an internal negative pressure filtration to obtain microspheres;

[0017] 5) After the electric push rod moves down and the filter frame loses the squeeze of the electric push rod, slide the filter frame to the bottom of the filter head, and wash the microspheres in the filter frame repeatedly 2-4 times with 250 ml of ethanol and deionized water respectively;

[0018] 6) The filter frame is sent into a vacuum drying oven by an L-shaped guide frame for low-temperature drying below 65 degrees Celsius to obtain liquid crystal microspheres with a core-shell structure.

[0019] Compared with the prior art, the present invention has the following advantages: a high-pressure mercury lamp is used in combination with an ultraviolet light initiator to achieve rapid polymerization of polymerizable monomers; since the intensity of ultraviolet light transmission has a gradient decrease, the polymerizable monomers will exhibit polymerization speed characteristics depending on the intensity of the ultraviolet light; during the stirring process, a core-shell structured microsphere liquid crystal can be quickly obtained, making the application of liquid crystal more flexible; and at the same time, the number of spacer microspheres added to the liquid crystal screen can be reduced.

[0020] The integrated design of the reaction bottle, funnel, liquid storage glass bottle and vacuum drying oven eliminates the need for frequent replacement of equipment during the preparation process, speeding up the preparation efficiency and simplifying the operation process. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention.

[0022] Figure 2 It is a schematic diagram of the three-dimensional structure from another viewing angle of the present invention.

[0023] Figure 3 It is a partial three-dimensional structural schematic diagram of the present invention.

[0024] Figure 4 It is a schematic diagram of the three-dimensional structure of the present invention after removing the transparent insulation box.

[0025] Figure 5 It is a schematic diagram of the three-dimensional structure of the reaction bottle, the motor and the glass stopper rod of the present invention.

[0026] Figure 6 It is a schematic diagram of the three-dimensional structure of the motor, bottle cap and stirrer of the present invention.

[0027] Figure 7 It is a schematic diagram of the three-dimensional structure of the glass stopper rod of the present invention.

[0028] Figure 8 It is a schematic diagram of the three-dimensional structure of the filter frame of the present invention.

[0029] Fig. 9 It is a schematic diagram of the three-dimensional structure of the vacuum drying box and the liquid storage box of the present invention.

[0030] Among them, the above-mentioned drawings include the following figure marks: 1, bottom plate, 2, liquid storage glass bottle, 3, funnel, 4, exhaust interface, 5, electric push rod, 6, vacuum drying oven, 7, transparent insulation box, 8, reaction bottle, 81, heating jacket, 82, high-pressure mercury lamp, 83, motor, 831, agitator, 84, glass stopper rod, 85, bottle cap, 9, ring-shaped cover plug, 10, ring-shaped plug, 11, L-shaped guide frame, 111, partition, 12, filter frame, 13, liquid storage tank, 131, catheter, 132, filter head. DETAILED DESCRIPTION

[0031] Although the present invention may be described with respect to a particular application or industry, those skilled in the art will recognize the broader applicability of the present invention. Those of ordinary skill in the art will recognize that terms such as above, below, upward, downward, etc. are used to describe the drawings and do not represent limitations on the scope of the present invention as defined by the appended claims. Any numerical designations such as first or second are merely exemplary and are not intended to limit the scope of the present invention in any way.

[0032] Example 1

[0033] A device and method for preparing LCD microspheres, such as Figure 1-Figure 3 , Figure 8 As shown, it includes a base plate 1, a liquid storage glass bottle 2, a funnel 3, an electric push rod 5, a vacuum drying box 6, a transparent insulation box 7, a reaction bottle 8 and a high-pressure mercury lamp 82. The liquid storage glass bottle 2 is placed on the base plate 1. An exhaust interface 4 is provided on the liquid storage glass bottle 2 for docking with an external exhaust fan. The mouth of the liquid storage glass bottle 2 is fixedly connected to the funnel 3, and the connection is liquid-sealed. Four electric push rods 5 are evenly distributed around the liquid storage glass bottle 2 on the base plate 1. The movable rod of the electric push rod 5 is fixedly connected to the funnel 3. The funnel 3 rises with the movable rod of the electric push rod 5 and the liquid storage glass bottle 2 rises together. A vacuum drying box 6 is installed on the right side of the base plate 1. A transparent insulation box 7 is fixedly connected to the base plate 1 by using a vertical rod as a support. The reaction bottle 8 is placed in the transparent insulation box 7. A high-pressure mercury lamp 82 is installed on the side of the transparent insulation box 7 close to the reaction bottle 8.

[0034] like Figure 1 , Figure 4 As shown, a heating jacket 81 is also included. The heating jacket 81 is installed at the bottom of the reaction bottle 8. The heating jacket 81 surrounds the bottom of the reaction bottle 8 and uses a temperature control module to adjust the heating power.

[0035] like Figure 1 , Figure 4As shown, it also includes a motor 83, an agitator 831 and a bottle cap 85. The bottle cap 85 is screwed on the top of the reaction bottle 8, and the motor 83 is installed on the bottle cap 85. The motor 83 adopts a 90mm industrial-grade DC brushless motor. The output shaft of the motor 83 is connected to the agitator 831, and the connection between the agitator 831 and the bottle cap 85 is connected by a shaft seal.

[0036] like Figure 1 , Figure 3 As shown, an annular plug 9 is also included. A feeding port is opened on the bottle cap 85, and the feeding port is closed by the annular plug 9. When the stirrer 831 is stirring, the annular plug 9 can prevent impurities from entering.

[0037] like Figure 3 , Figure 5 , Figure 7 As shown, a glass stopper rod 84 is also included. A circular hole is opened at the bottom of the reaction bottle 8. The circular hole protrudes and passes through the bottom of the transparent insulation box 7. The glass stopper rod 84 is slidably placed in the circular hole. A rubber pad is provided at the contact position between the glass stopper rod 84 and the circular hole to achieve a leak-proof effect. The glass stopper rod 84 falls due to the generated gravity and maintains a closed circular hole state.

[0038] like Figure 1 , Fig. 9 As shown, it also includes an L-shaped guide frame 11, a partition 111 and a filter frame 12. A notch is opened on the vacuum drying box 6, and the two sides of the notch are fixedly connected to the L-shaped guide frames 11 opposite to each other. The right side of the L-shaped guide frame 11 extends to the inside of the vacuum drying box 6, and the left side extends to the bottom of the transparent insulation box 7. The filter frame 12 is slidably connected to the L-shaped guide frame 11, and the partition 111 is slidably connected at the notch. The partition 111 slides up and down and is airtightly connected to the notch. The filter frame 12 can be airtightly attached to the bottom of the transparent insulation box 7 as the funnel 3 moves upward. The filter in the filter frame 12 will lift the glass stopper rod 84, so that the glass stopper rod 84 and the circular hole at the bottom of the reaction bottle 8 are separated, so that the liquid in the reaction bottle 8 flows into the filter frame 12.

[0039] like Figure 1 , Figure 4 As shown, an annular plug 10 is also included. The annular plug 10 is welded to the bottom of the transparent insulation box 7, and the annular plug 10 surrounds the glass plug rod 84 that has passed through. A circular groove is opened on the filter frame 12. During the upward movement of the filter frame 12, the circular groove and the annular plug 10 are in airtight fit.

[0040] like Figure 1 , Fig. 9As shown, it also includes a liquid storage tank 13, a conduit 131 and a filter head 132. The vacuum drying box 6 and the transparent insulation box 7 are fixedly connected with the liquid storage tank 13. The liquid storage tank 13 is used to store the solution required for washing. The bottom of the liquid storage tank 13 is connected to the conduit 131. The filter head 132 is arranged at the bottom of the conduit 131. The filter head 132 can reduce the liquid flow rate. The filter head 132 is located above the L-shaped guide frame 11. The filter frame 12 can slide to the bottom of the filter head 132 through the L-shaped guide frame 11.

[0041] The method for preparing LCD microspheres comprises the following steps:

[0042] 1) 1000 g of water, 0.78 g of hydroxyethyl cellulose, 0.2 g of tricalcium phosphate and 0.06 g of polyvinyl pyrrolidone were added to a 5-liter reaction bottle 8, wherein polyvinyl pyrrolidone is used as a dispersing and suspending medium to accelerate the nucleation speed and make the particle size distribution more uniform. At the same time, 540 g of pentaerythritol tetraacrylate and 1250 g of liquid crystal STNBSR72700-000 (produced by Beijing Bayi Spacetime Liquid Crystal Technology Co., Ltd.) were added, wherein pentaerythritol tetraacrylate contains 25% of 1,6-hexanediol acrylate, 4.3% of UV absorber UVP-327, 3.6% of UV photoinitiator 907 and 0.3% of tert-butyl peroxybenzoate;

[0043] 2) Turn on the high-pressure mercury lamp 82 to irradiate the reaction bottle 8, so that the ultraviolet light intensity on the bottle surface is 2.8 mW / cm2. The ultraviolet wavelength of the high-pressure mercury lamp 82 combined with the ultraviolet light initiator 907 can accelerate the polymerization speed, thus reducing the reaction waiting time;

[0044] 3) Cover the bottle cap 85 and place the stirrer 831 in the reaction bottle 8. The temperature of the heating jacket 81 is controlled at 96 degrees Celsius and the stirrer 831 starts stirring. The speed of the motor 83 is maintained at 3200 rpm. Keep the temperature at this temperature for 6 hours and wait for the reaction.

[0045] 4) After the reaction is completed, filter paper is placed on the filter frame 12, and the electric push rod 5 is started to move the funnel 3 and the liquid storage glass bottle 2 upward. The funnel 3 fits the bottom of the filter frame 12, and the annular plug 10 is inserted into the circular groove on the filter frame 12. After the funnel 3, the filter frame 12 and the annular cover plug 9 are in close contact, the filter frame 12 lifts the glass plug rod 84, and the mixed liquid in the reaction bottle 8 flows into the filter frame 12. The air extraction interface 4 of the liquid storage glass bottle 2 is connected to the vacuum pump, and the annular cover plug 9 is opened. The vacuum pump extracts air from the liquid storage glass bottle 2 to form an internal negative pressure filtration to obtain microspheres;

[0046] 5) After the electric push rod 5 moves downward and the filter frame 12 loses the squeezing of the electric push rod 5, the filter frame 12 is pushed to slide to the bottom of the filter head 132, and the microspheres in the filter frame 12 are repeatedly washed 3 times with 250 ml of ethanol and deionized water respectively to remove the residual impurities attached to the surface of the microspheres in preparation for purification;

[0047] 6) The filter frame 12 is sent into the vacuum drying oven 6 by the L-shaped guide frame 11 and dried at 50 degrees Celsius for 3 hours to obtain pure liquid crystal microspheres with a core-shell structure.

[0048] The above embodiments are provided for persons familiar with the art to implement or use the present invention. Personnel familiar with the art can make various modifications or changes to the above embodiments without departing from the inventive concept of the present invention. Therefore, the protection scope of the present invention is not limited to the above embodiments, but should be the maximum scope of the innovative features mentioned in the claims.

Claims

1. A device for preparing LCD microspheres, comprising: A bottom plate (1), a liquid storage glass bottle (2), a funnel (3), an electric push rod (5), a vacuum drying box (6), a transparent heat preservation box (7), a reaction bottle (8) and a high-pressure mercury lamp (82) are provided. The liquid storage glass bottle (2) is placed on the bottom plate (1). The mouth of the liquid storage glass bottle (2) is fixedly connected to the funnel (3). The electric push rods (5) are evenly distributed and installed on the bottom plate (1). The movable rods of the electric push rods (5) are fixedly connected to the funnel (3). A vacuum drying box (6) is installed on one side of the bottom plate (1). The transparent heat preservation box (7) is fixedly connected to the bottom plate (1) via a vertical rod. The reaction bottle (8) is placed in the transparent heat preservation box (7). The high-pressure mercury lamp (82) is installed on one side of the transparent heat preservation box (7) close to the reaction bottle (8). The liquid storage glass bottle (2) is provided with an air extraction interface (4) for connecting to an external air extraction machine; The funnel (3) rises along with the movable rod of the electric push rod (5), and the liquid storage glass bottle (2) rises along with it; It also includes a glass stopper rod (84). A circular hole is opened at the bottom of the reaction bottle (8). The circular hole protrudes and passes through the bottom of the transparent insulation box (7). The glass stopper rod (84) is slidably placed in the circular hole. The glass stopper rod (84) falls due to gravity to keep the circular hole closed. The invention also comprises an L-shaped guide frame (11), a partition (111) and a filter frame (12); a notch is formed on the vacuum drying box (6); two sides of the notch are fixedly connected to the L-shaped guide frames (11) which are opposite to each other; the filter frame (12) is slidably connected to the L-shaped guide frame (11); the notch is slidably connected to the partition (111); the partition (111) slides up and down and is airtightly connected to the notch; the filter frame (12) can be airtightly attached to the bottom of the transparent insulation box (7) as the funnel (3) moves upward; the filter in the filter frame (12) lifts the glass stopper rod (84), so that the glass stopper rod (84) and the circular hole at the bottom of the reaction bottle (8) are separated, thereby allowing the liquid in the reaction bottle (8) to flow into the filter frame (12).

2. The LCD microsphere preparation device according to claim 1, characterized in that: It also includes a heating jacket (81), and the heating jacket (81) is installed at the bottom of the reaction bottle (8).

3. The LCD microsphere preparation device according to claim 2, characterized in that: The invention also comprises a motor (83), an agitator (831) and a bottle cap (85); the bottle cap (85) is screwed onto the top of the reaction bottle (8); the motor (83) is mounted on the bottle cap (85); and the output shaft of the motor (83) is connected to the agitator (831).

4. The LCD microsphere preparation device according to claim 3, characterized in that: It also includes an annular cover plug (9), and a feeding port is formed on the bottle cap (85), and the feeding port is closed by the annular cover plug (9).

5. The LCD microsphere preparation device according to claim 4, characterized in that: It also includes an annular plug (10), the annular plug (10) being fixedly connected to the bottom of the transparent heat preservation box (7) and surrounding the protruding glass plug rod (84), and a circular groove being formed on the filter screen frame (12), the circular groove and the annular plug (10) being airtightly fitted.

6. The LCD microsphere preparation device according to claim 5, characterized in that: The invention also comprises a liquid storage box (13), a conduit (131) and a filter head (132); the vacuum drying box (6) and the transparent heat preservation box (7) are fixedly connected to the liquid storage box (13); the bottom of the liquid storage box (13) is connected to the conduit (131); the bottom of the conduit (131) is provided with a filter head (132); and the filter head (132) is arranged above the L-shaped guide frame (11).

7. A device for preparing LCD microspheres according to any one of claims 1 to 6, characterized in that: The invention also includes a method for preparing LCD microspheres, the steps of which are as follows: 1) Add water, hydroxyethyl cellulose, tricalcium phosphate and polyvinyl pyrrolidone in a ratio of 50000:39:10:3 into a reaction bottle (8), wherein polyvinyl pyrrolidone is used as a dispersing and suspending medium, and simultaneously add 0.5-0.55 times the mass of water of pentaerythritol tetraacrylate and 1.2-1.3 times the mass of water of liquid crystal, wherein pentaerythritol tetraacrylate contains 25% 1,6-hexanediol acrylate, 4.3% ultraviolet absorber, 3.6% ultraviolet photoinitiator and 0.3% tert-butyl peroxybenzoate; 2) Turn on the high pressure mercury lamp (82) to irradiate the reaction bottle (8); 3) Cover the bottle cap (85) and place the stirrer (831) in the reaction bottle (8), control the temperature of the heating jacket (81) to between 90 and 110 degrees Celsius and start stirring with the stirrer (831); 4) After the reaction is completed, filter paper is placed on the filter frame (12), and the electric push rod (5) is started to move the funnel (3) and the liquid storage glass bottle (2) upward. The funnel (3) fits the bottom of the filter frame (12), and the annular plug (10) is inserted into the circular groove on the filter frame (12). After the funnel (3), the filter frame (12) and the annular cover plug (9) are in close contact, the filter frame (12) lifts the glass plug rod (84), and the mixed liquid in the reaction bottle (8) flows into the filter frame (12). The exhaust interface (4) of the liquid storage glass bottle (2) is connected to the exhaust machine, and the annular cover plug (9) is opened. The exhaust machine exhausts the liquid storage glass bottle (2) to form an internal negative pressure filtration to obtain microspheres; 5) The electric push rod (5) moves downward, and after the filter frame (12) loses the squeezing of the electric push rod (5), the filter frame (12) is moved to slide below the filter head (132), and the microspheres in the filter frame (12) are repeatedly washed 2-4 times with 250 ml of ethanol and deionized water respectively; 6) The filter frame (12) is sent into a vacuum drying oven (6) by the L-shaped guide frame (11) for low-temperature drying at a temperature below 65 degrees Celsius to obtain liquid crystal microspheres with a core-shell structure.

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