阅读说明：本技术 一种液晶树脂填充剂微球二氧化硅的制备方法 (Preparation method of liquid crystal resin filler microsphere silicon dioxide ) 是由 余惠华 卢元方 陈家茂 于 2020-06-18 设计创作，主要内容包括：本发明涉及无机材料技术领域,尤其涉及一种液晶树脂填充剂二氧化硅的制备方法。通过以白油、氨水、硅酸钠作为原料,水解获得二氧化硅,然后再经过熟化,过滤后配制获得二氧化硅浆料,再加入渗透剂反应,过滤,煅烧后冷却获得微球状二氧化硅,采用该方法制备的二氧化硅可用于反射膜及防反射膜中,起到较好的效果。(The invention relates to the technical field of inorganic materials, in particular to a preparation method of liquid crystal resin filler silicon dioxide. White oil, ammonia water and sodium silicate are used as raw materials, silicon dioxide is obtained through hydrolysis, then the silicon dioxide is cured and filtered to prepare silicon dioxide slurry, a penetrating agent is added for reaction, the silicon dioxide is filtered and calcined, and then the microspherical silicon dioxide is obtained through cooling.)

1. A preparation method of liquid crystal resin filler microsphere silicon dioxide is characterized by comprising the following steps:

the method specifically comprises the following steps:

(1) preparing raw materials: adding water into sodium silicate to prepare aqueous solution with the density of 1.2-1.3 g/ml; preparing raw materials of white oil and 20wt% of ammonia water for later use;

(2) synthesizing: adding white oil into a reaction kettle, adding the sodium silicate prepared in the step (1), starting stirring at a rotating speed of 150-200 rpm, and reacting at a certain temperature and under a certain pH condition;

(3) curing: heating the material reacted in the step (2) for reaction;

(4) washing with water: filtering the cured material in the step (3), adding hot water at 50-60 ℃ to prepare slurry of 15-20wt% of silicon dioxide, adding a penetrating agent JFC, stirring at the rotating speed of 60-80 rpm, stirring for 20-30 minutes, filtering, and then adding deionized water at 30-40 ℃ for continuous washing;

(5) and (3) calcining: and (4) calcining the material obtained in the step (4), cooling to normal temperature, and discharging to obtain the microspherical silicon dioxide.

2. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the white oil in the step (1) is selected from refined white oil of Shandong star chemical plants.

3. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the adding amount of the white oil in the step (2) is calculated according to the volume ratio: white oil: sodium silicate = 1-1.5.

4. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the reaction conditions in the step (2) are as follows: dropping ammonia water at 40-50 deg.C to maintain pH 8-9, and reacting at this temperature for 4-5 hr.

5. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the heating reaction in the step (3) is specifically as follows: heating to 80-90 deg.c and maintaining for 1-2 hr.

6. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: in the step (4), the addition amount of the penetrating agent JFC is 0.5-1wt% of the mass of the silicon dioxide slurry.

7. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the resistivity of the washing water in the step (4) is less than 50 omega/cm.

8. The method for preparing silica microspheres for liquid crystal resin fillers according to claim 1, wherein the method comprises the following steps: the calcination in the step (5) is as follows: calcining at 550-600 deg.C, and keeping the temperature for 3-4 hr.

9. A liquid crystal resin filler microsphere silica prepared according to the process of any one of claims 1 to 8, wherein: the diameter of the microsphere silicon dioxide is 2-5 microns.

Technical Field

The invention relates to the technical field of inorganic materials, in particular to a preparation method of liquid crystal resin filler silicon dioxide.

Background

In the flat panel display industry, LCD liquid crystal displays with high image quality and low power consumption are becoming mainstream products in the market. The liquid crystal display utilizes the property that the liquid crystal display changes its optical properties by causing molecular rearrangement under the action of an electric field. However, the display device itself is a non-self-luminous display device, and an optical functional film is used in combination to convert such optical change into image display. The liquid crystal display film comprises a polarizing film, a protective film optical compensation film and a backlight film, and the reflecting film in the backlight film component plays an important role in improving the performance of the liquid crystal display and reducing the energy consumption. With the increase in size, weight, and thickness of liquid crystal televisions, L is required to have higher mechanical strength, dimensional stability, heat dissipation, and the like.

The preparation method of the reflecting film comprises the following steps: multilayer stacking methods, foaming methods, and blending methods. The blending method has low cost and easy processing, and is suitable for being used as a reflecting film of a large-size liquid crystal display.

The reflective film can be classified into a PE film and a PC film according to the material, and the PC reflective film has advantages of high heat resistance, good mechanical properties, light weight, low processing cost, and the like, and has attracted much attention in recent years. However, the reflectivity of the existing domestic PC reflective film is still a certain gap compared with that of foreign products. How to improve the performance of the liquid crystal film is a problem to be solved in the field of liquid crystal display at present.

The main inorganic filler of the liquid crystal reflecting film is titanium dioxide, however, only titanium dioxide is added to a large LCD liquid crystal display to meet the requirements of strength and dimensional stability of the film, therefore, a preparation method of the liquid crystal resin filler silicon dioxide is invented, and the silicon dioxide prepared by the method can be used in the reflecting film and the anti-reflection film to achieve a better effect.

Disclosure of Invention

The invention aims to provide a preparation method of liquid crystal resin filler microsphere silicon dioxide. The invention takes sodium silicate as raw material, and prepares microspherical silicon dioxide by processes of polymerization, modification and the like, and adopts the following technical scheme for realizing the purpose:

a preparation method of liquid crystal resin filler microsphere silicon dioxide specifically comprises the following steps:

(1) preparing materials: adding water into sodium silicate to prepare aqueous solution with the density of 1.2-1.3 g/ml; white oil and ammonia water (20 wt%) for later use;

(2) synthesizing: adding white oil into a reaction kettle, adding prepared sodium silicate, starting stirring at a rotating speed of 150-200 r/min, dropwise adding ammonia water at 40-50 ℃ to keep the pH value at 8-9, and reacting at the temperature for 4-5 hours;

(3) curing: heating the hydrolyzed material in the step (2) to 80-90 ℃, and preserving heat for 1-2 hours.

(4) Washing with water: filtering the cured material in the step (3), adding hot water at 50-60 ℃ to prepare slurry with 15-20wt% of silicon dioxide, adding a penetrating agent JFC, stirring at the rotating speed of 60-80 rpm, stirring for 20-30 minutes, filtering, adding deionized water at 30-40 ℃ and continuously washing, wherein the washing water resistivity is less than 50 omega/cm.

(5) And (3) calcining: and (4) calcining the material obtained in the step (4) at 550-600 ℃, preserving heat for 3-4 hours, cooling to normal temperature, and discharging to obtain 2-5 micron spherical silicon dioxide.

Further, the white oil in the step (1) is selected from refined white oil of Shandong Xinchen chemical plant;

further, the adding amount of the white oil in the step (2) is that: sodium silicate =1-1.5 (by volume);

further, the addition amount of the penetrating agent JFC in the step (4) is 0.5-1% of that of the silicon dioxide.

The invention has the following remarkable advantages:

(1) the microsphere silicon dioxide product prepared by the invention has good sphericity, diameter of 2-5 microns, stable chemical property, narrow particle size distribution and uniform particle size; the application of the method in PE anti-reflection films improves the extinction efficiency and greatly improves the extinction performance.

(2) The method has short production period, can obtain the silicon dioxide gas microspheres within 24 hours, greatly reduces the production cost and makes large-scale production and application possible.

Drawings

FIG. 1 is a graph showing the particle size distribution of the microspheroidal silica product prepared according to the present invention.

Detailed Description

For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.