A method for preparing a brown glass bottle for storing adhesives

Abstract

This invention relates to a method for preparing a brown glass bottle for storing adhesives, characterized by: (1) acid treatment of the inner surface of the glass bottle, adding a Tris-HCl solution with pH=8~9 and 50~100g of dopamine into the bottle, stirring and mixing, washing and drying to obtain a glass bottle with black polydopamine grafted onto the inner surface; (2) activation of the surface of nano-inorganic particles, adding 20~30 drops of silane coupling agent to an ethanol aqueous solution for hydrolysis reaction, then adding 50~100g of surface-activated nano-inorganic particles for stirring, washing and drying to obtain nano-inorganic particles grafted with silane coupling agent; (3) preparing an acid / alkali solution with pH>4 in the glass bottle with black polydopamine grafted onto the inner surface, adding 10~50g of nano-inorganic particles grafted with silane coupling agent, stirring and reacting, washing and drying to obtain a black glass bottle with nano-inorganic particles deposited on the surface. Advantages of this invention: simple preparation method and convenient operation; it can produce a type of adhesive storage bottle that can block light and control the precipitation of metal ions.

Description

Technical Field

[0001] This invention belongs to the field of glass preparation technology and relates to a method for preparing a brown glass bottle for storing adhesives. Background Technology

[0002] Some adhesive products on the market have complex compositions and are prone to aging under light. Even extremely small particles can alter their composition, affecting their effectiveness. These adhesives require extremely stringent packaging and storage materials.

[0003] Glass, due to its excellent optical, mechanical, thermal, and chemical stability properties, is a superior material for the storage and packaging of adhesives. To meet the light-protection requirements of certain adhesives, brown glass bottles are commonly used for storage. Compared to transparent glass bottles, their application range is narrower, and their manufacturing process is more complex. Furthermore, to control the precipitation of metal ions after long-term contact between glass and adhesives, the inner surface of the glass bottle is coated with a film of nano-inorganic particles (silicon dioxide, titanium dioxide, etc.). However, untreated nano-inorganic particles are prone to agglomeration, which greatly affects the uniformity of the nano-inorganic particle film. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the existing technology and provide a method for preparing a brown glass bottle for storing adhesives.

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

[0006] A method for preparing a brown glass bottle for storing adhesives, characterized by comprising the following steps:

[0007] (1) Treat the inner surface of the glass bottle with acid, then prepare a Tris-HCl (pH=8~9) solution, add the Tris-HCl solution to the acid-treated glass bottle, then weigh dopamine and add it to the Tris-HCl solution, controlling the amount of dopamine added to be 50~100g, stir and mix to allow it to react, wash and dry after the reaction to obtain a glass bottle with black polydopamine grafted on the inner surface;

[0008] (2) The surface of the nano-inorganic particles is activated, and then an ethanol aqueous solution is prepared. A silane coupling agent is added to the ethanol aqueous solution to carry out a hydrolysis reaction. The amount of silane coupling agent added is controlled to be 20-30 drops. After the reaction is completed, the surface-activated nano-inorganic particles are added to the hydrolysate and stirred. The amount of surface-activated nano-inorganic particles added is controlled to be 50-100g. The particles are washed and dried to obtain nano-inorganic particles grafted with silane coupling agent.

[0009] (3) In the glass bottle with black polydopamine grafted on the inner surface obtained in step (1), an acid / base solution with pH > 4 is prepared. Nano-inorganic particles with grafted silane coupling agent are added to the solution. The amount of nano-inorganic particles with grafted silane coupling agent is controlled to be 10~50g. An electrostatic transfer reaction occurs by stirring. The solution is washed and dried to obtain a black glass bottle with nano-inorganic particles deposited on the surface.

[0010] Furthermore, the acid used in the glass bottle acid treatment in step (1) is a mixed acid, which is a mixture of hydrofluoric acid, concentrated sulfuric acid and hydrochloric acid in a volume ratio of 1:(2~5):(2~5).

[0011] Furthermore, the stirring time in steps (1) and (2) is 5 to 10 hours.

[0012] Furthermore, the nano-inorganic particles in step (2) are any one of silicon dioxide, hexagonal boron nitride, titanium dioxide, etc.

[0013] Furthermore, the method for surface activation of nano-inorganic particles in step (2) is as follows: prepare 10~15mol / L concentrated hydrochloric acid or 3~10mol / L sodium hydroxide, add 20~300g of silicon dioxide, titanium dioxide or hexagonal boron nitride, react in an oil bath at 100~200℃ for 5~10h, then wash repeatedly with ethanol and water 2~5 times, and dry in an oven at 80~100℃.

[0014] Furthermore, in step (2), the volume ratio of ethanol to water in the ethanol-water solution is (8~10):1.

[0015] Furthermore, the silane coupling agent in step (2) is one of KH550, KH570, DC5700, etc.

[0016] Furthermore, the hydrolysis method in step (2) is to stir for 5 to 30 minutes at 40 to 60°C.

[0017] Furthermore, the stirring conditions in step (3) are 10~24h and 40~60℃.

[0018] Furthermore, the washing steps in steps (1), (2), and (3) are as follows: wash the glass bottle with ethanol and water 2 to 5 times respectively until the ethanol or water after washing is transparent.

[0019] Furthermore, the drying conditions in steps (1), (2), and (3) are: drying at 50~100℃.

[0020] This invention first activates the surface of a transparent glass bottle with acid, then deposits a layer of black polydopamine (PDA), and simultaneously treats nano-inorganic particles (silicon dioxide, hexagonal boron nitride, titanium dioxide, etc.) with a silane coupling agent (DC5700). Through electrostatic transfer, the nano-inorganic particle film is uniformly coated on the inner surface of the glass bottle, and finally a gel storage product with a uniformly dispersed nano-inorganic particle film on the inner surface is prepared.

[0021] The beneficial effects of this invention are:

[0022] The preparation method of this invention is simple and easy to operate; the bottle body is treated with dopamine (DA) to achieve a light-blocking effect, and at the same time, the nano-inorganic particles are treated with silane coupling agent to enhance the uniformity of the nano-inorganic particle (silicon dioxide, hexagonal boron nitride, titanium dioxide) film, thereby preparing a gel storage bottle that can block light and control the precipitation of metal ions. Attached Figure Description

[0023] Figure 1 SEM images of uncoated and coated glass;

[0024] Figure 2 SEM image of glass coated with nano-SiO2 particle film;

[0025] Figure 3 SEM image of glass coated with h-BNNS particulate film;

[0026] Figure 4 SEM image of glass coated with nano-TiO2 particle film;

[0027] Figure 5 The transmittance diagrams are for uncoated and coated glass, from... Figure 5 It can be clearly seen that the transmittance of the glass bottle prepared by the present invention is significantly lower than that of transparent glass, thus achieving a light-blocking effect. Detailed Implementation

[0028] The invention will be further described below with reference to the accompanying drawings:

[0029] A method for preparing a brown glass bottle for storing adhesives, the specific implementation steps of which are as follows: Example

[0030] (1) The inner surface of the glass bottle was treated with 1L of mixed acid (made by mixing hydrofluoric acid, concentrated sulfuric acid and hydrochloric acid = 1:3:3). Then, 1L of Tris-HCl (pH=8.5) solution was prepared and added to the acid-treated glass bottle. Then, 50g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 5h, the glass bottle was washed 3 times with ethanol and water respectively until the ethanol or water after washing was transparent. Then, it was placed in a 50℃ oven and dried for 5h to obtain a glass bottle with black polydopamine grafted on the inner surface.

[0031] (2) Prepare 1L of 10mol / L concentrated hydrochloric acid, add 20g of silicon dioxide, react in an oil bath at 120℃ for 5h, then wash repeatedly with ethanol and water 3 times, and dry in an oven at 80℃ for 10h to activate the surface of the nano silicon dioxide particles. Then prepare 1L of ethanol aqueous solution (ethanol and water are mixed at a volume ratio of 9:1), and add 25 drops of silane coupling agent KH550 to the ethanol aqueous solution. Stir at 40℃ for 5min to hydrolyze it. After the reaction is completed, add 50g of surface-activated nano inorganic particles to the hydrolysate and stir for 5h. Wash with ethanol and water 3 times respectively, and dry in an oven at 50℃ for 10h to obtain nano silicon dioxide particles grafted with silane coupling agent.

[0032] (3) Add 1L of dilute hydrochloric acid solution with pH 5 to the glass bottle with black polydopamine grafted on the inner surface obtained in step (1), and then add 20g of nano silica particles grafted with silane coupling agent. Stir at 40°C for 10h to allow electrostatic transfer reaction to occur. Wash with ethanol and water three times respectively, and dry in an oven at 50°C for 10h to obtain a black glass bottle with nano silica particles deposited on the surface. Example

[0033] (1) The inner surface of the glass bottle was treated with 2L of mixed acid (made by mixing hydrofluoric acid, concentrated sulfuric acid and hydrochloric acid = 1:2:2). Then, 1L of Tris-HCl (pH=8) solution was prepared and added to the acid-treated glass bottle. Then, 80g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 8h, the glass bottle was washed 5 times with ethanol and water respectively until the ethanol or water after washing was transparent. Then, it was placed in an 80℃ oven and dried for 12h to obtain a glass bottle with black polydopamine grafted on the inner surface.

[0034] (2) Prepare 2L of 10mol / L sodium hydroxide, add 100g of nano hexagonal boron nitride particles, react in an oil bath at 180℃ for 10h, then wash repeatedly with ethanol and water 5 times, and dry in an oven at 80℃ for 10h to activate the surface of the nano hexagonal boron nitride particles. Then prepare 1L of ethanol aqueous solution (ethanol and water are mixed at a volume ratio of 8:1), and add 28 drops of silane coupling agent DC5700 to the ethanol aqueous solution. Stir at 55℃ for 10min to hydrolyze it. After the reaction is completed, add 80g of surface-activated nano hexagonal boron nitride particles to the hydrolysate and stir for 8h. Wash with ethanol and water 3 times respectively, and dry in an oven at 80℃ for 12h to obtain nano hexagonal boron nitride particles grafted with silane coupling agent.

[0035] (3) Add 1L of sodium hydroxide with pH 8 to the glass bottle with black polydopamine grafted on the inner surface obtained in step (1), and then add 50g of nano-hexagonal boron nitride particles grafted with silane coupling agent. Stir at 40°C for 10h to allow it to undergo an electrostatic transfer reaction. Wash with ethanol and water 5 times respectively, and dry in an oven at 80°C for 12h to obtain a black glass bottle with nano-hexagonal boron nitride particles deposited on the surface. Example

[0036] (1) The inner surface of the glass bottle was treated with 1.5L of mixed acid (made by mixing hydrofluoric acid, concentrated sulfuric acid and hydrochloric acid = 1:5:5). Then, 2L of Tris-HCl (pH=9) solution was prepared and added to the acid-treated glass bottle. Then, 100g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 10h, the glass bottle was washed 5 times with ethanol and water respectively until the ethanol or water after washing was transparent. Then, it was placed in a 100℃ oven and dried for 15h to obtain a glass bottle with black polydopamine grafted on the inner surface.

[0037] (2) Prepare 2L of 15mol / L concentrated hydrochloric acid, add 100g of nano titanium dioxide particles, react in an oil bath at 130℃ for 6h, then wash repeatedly with ethanol and water 5 times, dry in an oven at 100℃ for 15h to activate the surface of nano titanium dioxide particles, then prepare 2L of ethanol aqueous solution (ethanol and water are mixed at a volume ratio of 10:1), and add 25 drops of silane coupling agent to the ethanol aqueous solution to activate the surface of nano titanium dioxide particles, stir at 50℃ for 8min to hydrolyze it, after the reaction is completed, add 100g of surface-activated nano titanium dioxide particles to the hydrolysate and stir for 6h, wash with ethanol and water 3 times respectively, and dry in an oven at 100℃ for 15h to obtain nano titanium dioxide particles grafted with silane coupling agent;

[0038] (3) Add 1L of dilute hydrochloric acid with pH 6 to the glass bottle with black polydopamine grafted on the inner surface obtained in step (1), and then add 30g of nano titanium dioxide particles grafted with silane coupling agent. Stir at 50°C for 15h to allow electrostatic transfer reaction to occur. Wash with ethanol and water three times respectively, and dry in an oven at 100°C for 15h to obtain a black glass bottle with nano titanium dioxide particles deposited on the surface.

[0039] Following the methods described in steps 1-3, temperature resistance, acid resistance, and alkali resistance tests were conducted using the cross-cut adhesion test. The results are shown in Table 1. SEM analysis was performed on the acidified glass, as shown in... Figure 1 As shown. SEM tests were performed on uncoated glass and treated glass bottles, as shown. Figures 1-4 At the same time, transmittance tests were conducted, such as... Figure 5 .

Claims

1. A method for preparing a brown glass bottle for storing adhesives, characterized in that... Includes the following steps: (1) Treat the inner surface of the glass bottle with acid, then prepare a Tris-HCl solution with pH=8~9, add the Tris-HCl solution to the acid-treated glass bottle, then weigh dopamine and add it to the Tris-HCl solution, controlling the amount of dopamine added to be 50~100g, stir and mix to allow it to react, wash and dry after the reaction to obtain a glass bottle with black polydopamine grafted on the inner surface; (2) The surface of the nano-inorganic particles is activated, and then an ethanol aqueous solution is prepared. A silane coupling agent is added to the ethanol aqueous solution for hydrolysis reaction. The amount of silane coupling agent added is controlled to be 20-30 drops. After the reaction is completed, the surface-activated nano-inorganic particles are added to the hydrolysate and stirred. The amount of surface-activated nano-inorganic particles added is controlled to be 50-100g. The particles are washed and dried to obtain nano-inorganic particles grafted with silane coupling agent. The method for surface activation of nano-inorganic particles in step (2) is as follows: 10-15 mol / L concentrated hydrochloric acid or 3-10 mol / L sodium hydroxide is prepared, and 20-300g of silicon dioxide, titanium dioxide or hexagonal boron nitride is added. The particles are reacted in an oil bath at 100-200℃ for 5-10h, and then washed repeatedly with ethanol and water 2-5 times. The particles are then dried in an oven at 80-100℃. (3) In the glass bottle with black polydopamine grafted on the inner surface obtained in step (1), an acid / base solution with pH > 4 is prepared. Nano-inorganic particles with grafted silane coupling agent are added to the solution. The amount of nano-inorganic particles with grafted silane coupling agent is controlled to be 10~50g. An electrostatic transfer reaction occurs by stirring. The solution is washed and dried to obtain a black glass bottle with nano-inorganic particles deposited on the surface.

2. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The acid used in the glass bottle acid treatment in step (1) is a mixed acid, which is a mixture of hydrofluoric acid, concentrated sulfuric acid and hydrochloric acid in a volume ratio of 1:(2~5):(2~5).

3. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The nano-inorganic particles in step (2) are any one of silicon dioxide, hexagonal boron nitride, and titanium dioxide.

4. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: In step (2), the volume ratio of ethanol to water in the ethanol-water solution is (8~10):

1.

5. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The silane coupling agent in step (2) is one of KH550, KH570, and DC5700.

6. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The hydrolysis method in step (2) is to stir for 5 to 30 minutes at 40 to 60°C.

7. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The stirring conditions in step (3) are 10~24h and 40~60℃.

8. The method for preparing a brown glass bottle for storing adhesives according to claim 1, characterized in that: The washing steps in steps (1), (2), and (3) are as follows: wash the glass bottle with ethanol and water 2 to 5 times respectively until the ethanol or water after washing is transparent.

9. A method for preparing a brown glass bottle for storing adhesives according to any one of claims 1 to 8, characterized in that: The drying conditions in steps (1), (2), and (3) are: drying at 50~100℃.

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