Preparation method of brown glass bottle for glue storage

Abstract

The invention relates to a preparation method of a brown glass bottle for glue storage, which is characterized by comprising the following steps: (1) carrying out acid treatment on the inner surface of the glass bottle, adding a Tris-HCl solution with the pH value of 8-9 and 50-100g of dopamine into the bottle, stirring, mixing, washing and drying to obtain the glass bottle with the inner surface grafted with black polydopamine; (2) activating the surfaces of the nano inorganic particles, adding 20-30 drops of a silane coupling agent into an ethanol water solution to carry out hydrolysis reaction, then adding 50-100g of the surface-activated nano inorganic particles, stirring, washing and drying to obtain the nano inorganic particles grafted with the silane coupling agent; and (3) preparing an acid / alkali solution of which the pH value is greater than 4 in the glass bottle of which the inner surface is grafted with the black polydopamine, adding 10-50g of the nano inorganic particles grafted with the silane coupling agent, stirring for reaction, washing, and drying to obtain the black glass bottle of which the surface is deposited with the nano inorganic particles. The preparation method has the advantages that the preparation method is simple and convenient to operate; the glue storage bottle capable of keeping away from light and controlling metal ion precipitation can be manufactured.

Description

Technical Field

[0001] The invention belongs to the technical field of glass preparation, and relates to a method for preparing a brown glass bottle for storing glue. Background Art

[0002] Some glue products on the market currently have complex ingredients, are easily aged under light, and tiny particles can also change their ingredients, affecting their effectiveness. These glues are extremely demanding on the materials used for packaging and storage.

[0003] Glass is an excellent material for storing and packaging adhesives due to its excellent optical, mechanical, thermal and chemical properties. In order to meet the light-proof requirements of certain adhesives, brown glass bottles are commonly used for storage on the market. Compared with transparent glass bottles, their application range is narrower and the preparation process is more complicated. At the same time, in order to control the precipitation of metal ions after long-term contact between glass and adhesives, the inner surface of the glass bottle will be coated with a film of nano-inorganic particles (silicon dioxide, titanium dioxide, etc.). However, untreated nano-inorganic particles are very easy to agglomerate, which will greatly affect the uniformity of the nano-inorganic particle film. Summary of the invention

[0004] The purpose of the invention is to solve the deficiencies in the prior art and to provide a method for preparing a brown glass bottle for storing glue.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows: A method for preparing a brown glass bottle for storing glue, characterized by comprising the following steps: (1) The inner surface of the glass bottle is treated with an acid, and then a Tris-HCl (pH=8-9) solution is prepared, and the Tris-HCl solution is added to the acid-treated glass bottle, and then dopamine is weighed and added to the Tris-HCl solution, and the amount of dopamine added is controlled to be 50-100 g, and the mixture is stirred and mixed to react, and after the reaction, the mixture is washed and dried to obtain a glass bottle with a black polydopamine grafted on the inner surface; (2) Activating the surface of the nano-inorganic particles, and then preparing an ethanol aqueous solution, and adding a silane coupling agent to the ethanol aqueous solution for hydrolysis reaction, controlling the amount of the silane coupling agent added to be 20-30 drops, adding the surface-activated nano-inorganic particles to the hydrolyzate after the reaction is completed, stirring, controlling the amount of the surface-activated nano-inorganic particles added to be 50-100 g, washing, and drying to obtain nano-inorganic particles grafted with a silane coupling agent; (3) In the glass bottle with the black polydopamine grafted on the inner surface obtained in step (1), an acid / base solution with a pH value greater than 4 is prepared, and nano-inorganic particles grafted with a silane coupling agent are added thereto, wherein the amount of the nano-inorganic particles grafted with a silane coupling agent is controlled to be 10-50 g, an electrostatic transfer reaction is caused by stirring, and the solution is washed and dried to obtain a black glass bottle with nano-inorganic particles deposited on the surface.

[0006] Furthermore, the acid used for the acid treatment of the glass bottle in step (1) is a mixed acid, which is a mixture of hydrofluoric acid: concentrated sulfuric acid: hydrochloric acid in a volume ratio of 1: (2-5): (2-5).

[0007] Furthermore, the stirring time in step (1) and step (2) is 5 to 10 hours.

[0008] Furthermore, the nano inorganic particles in step (2) are any one of silicon dioxide, hexagonal boron nitride, titanium dioxide, etc.

[0009] Furthermore, the method for surface activation of the nano inorganic particles in step (2) is: prepare 10-15 mol / L concentrated hydrochloric acid or 3-10 mol / L sodium hydroxide, add 20-300 g of silicon dioxide, titanium dioxide or hexagonal boron nitride, react in an oil bath at 100-200° C. for 5-10 hours, then repeatedly wash with ethanol and water for 2-5 times, and dry in an oven at 80-100° C.

[0010] Furthermore, the volume ratio of ethanol to water in the ethanol-water solution in step (2) is (8-10):1.

[0011] Furthermore, the silane coupling agent in step (2) is one of kh550, kh570, DC5700 and the like.

[0012] Furthermore, the hydrolysis method in step (2) is to stir at 40-60° C. for 5-30 minutes.

[0013] Furthermore, the stirring conditions in step (3) are 10-24 hours and 40-60°C.

[0014] Furthermore, the washing step in step (1), step (2) and step (3) is: washing the glass bottle with ethanol and water for 2 to 5 times respectively until the ethanol or water after washing becomes transparent.

[0015] Furthermore, the drying conditions in step (1), step (2) and step (3) are: drying at 50-100°C.

[0016] The present invention first activates the surface of a transparent glass bottle with acid, then deposits a layer of black polydopamine (PDA), and simultaneously uses a silane coupling agent (DC5700) to treat nano inorganic particles (silicon dioxide, hexagonal boron nitride, titanium dioxide, etc.), and then uses electrostatic transfer to evenly coat the nano inorganic particle film on the inner surface of the glass bottle, and finally prepares a glue storage having a uniformly dispersed nano inorganic particle film on the inner surface.

[0017] Beneficial effects of the present invention: The preparation method of the invention is simple and easy to operate; dopamine (DA) is used to treat the bottle body to achieve a light-proof effect, and a silane coupling agent is used to treat the nano-inorganic particles to enhance the uniformity of the nano-inorganic particle (silicon dioxide, hexagonal boron nitride, titanium dioxide) film, thereby preparing a glue storage bottle that can avoid light and control the precipitation of metal ions. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 The SEM images of uncoated glass and coated glass; Figure 2 This is the SEM image of glass coated with nano-SiO2 particle film; Figure 3 This is the SEM image of glass coated with h-BNNS particle film; Figure 4 This is the SEM image of glass coated with nano-TiO2 particle film; Figure 5 is the transmittance diagram of uncoated glass 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, and the light-shielding effect can be achieved. DETAILED DESCRIPTION

[0019] The present invention will be further described below in conjunction with the accompanying drawings: A method for preparing a brown glass bottle for storing glue, the specific implementation steps are as follows: Example

[0020] (1) The inner surface of the glass bottle was treated with 1L of mixed acid (mixed with hydrofluoric acid: concentrated sulfuric acid: hydrochloric acid = 1:3:3), and then 1L of Tris-HCl (pH = 8.5) solution was prepared. The Tris-HCl solution was added to the acid-treated glass bottle, and then 50g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 5 hours, the glass bottle was washed with ethanol and water for 3 times respectively until the ethanol or water after washing was transparent, and then placed in a 50°C oven for drying for 5 hours to obtain a glass bottle with a black polydopamine grafted on the inner surface; (2) Prepare 1L of 10mol / L concentrated hydrochloric acid, add 20g of silica, react in an oil bath at 120°C for 5h, then wash repeatedly with ethanol and water for 3 times, dry in an oven at 80°C for 10h to activate the surface of the nano-silica particles, then prepare 1L of ethanol aqueous solution (ethanol and water are mixed in a volume ratio of 9:1), and drop 25 drops of silane coupling agent kh550 into the ethanol aqueous solution, stir for 5min at 40°C to hydrolyze it, add 50g of surface-activated nano-inorganic particles to the hydrolyzate after the reaction is completed, stir for 5h, wash with ethanol and water for 3 times respectively, and dry in an oven at 50°C for 10h to obtain nano-silica particles grafted with silane coupling agent; (3) Add 1 L of dilute hydrochloric acid solution with a pH of 5 into the glass bottle with the inner surface grafted with black polydopamine obtained in step (1), then add 20 g of nano-silica particles grafted with a silane coupling agent, stir at 40° C. for 10 h to allow an electrostatic transfer reaction to occur, wash with ethanol and water three times respectively, and dry in an oven at 50° C. for 10 h to obtain a black glass bottle with nano-silica particles deposited on the surface. Example

[0021] (1) The inner surface of the glass bottle was treated with 2L of mixed acid (mixed with hydrofluoric acid: concentrated sulfuric acid: hydrochloric acid = 1:2:2), and then 1L of Tris-HCl (pH = 8) solution was prepared. The Tris-HCl solution was added to the acid-treated glass bottle, and then 80g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 8 hours, the glass bottle was washed with ethanol and water for 5 times respectively until the ethanol or water after washing was transparent, and then placed in an oven at 80°C for 12 hours to obtain a glass bottle with a black polydopamine grafted on the inner surface; (2) Prepare 2L of 10mol / L sodium hydroxide, add 100g of nano hexagonal boron nitride particles, react in an oil bath at 180°C for 10h, then wash with ethanol and water repeatedly for 5 times, dry in an oven at 80°C 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 in a volume ratio of 8:1), and drop 28 drops of silane coupling agent DC5700 into the ethanol aqueous solution, stir for 10min at 55°C to hydrolyze it, add 80g of surface-activated nano hexagonal boron nitride particles to the hydrolyzate after the reaction is completed, stir for 8h, wash with ethanol and water for 3 times respectively, and dry in an oven at 80°C for 12h to obtain nano hexagonal boron nitride particles grafted with silane coupling agent; (3) Add 1 L of sodium hydroxide with a pH of 8 into the glass bottle with the inner surface grafted with black polydopamine obtained in step (1), and then add 50 g of nano hexagonal boron nitride particles grafted with a silane coupling agent, stir at 40° C. for 10 h to allow an electrostatic transfer reaction to occur, wash with ethanol and water for 5 times respectively, and dry in an oven at 80° C. for 12 h to obtain a black glass bottle with nano hexagonal boron nitride particles deposited on the surface. Example

[0022] (1) The inner surface of the glass bottle was treated with 1.5 L of mixed acid (mixed with hydrofluoric acid: concentrated sulfuric acid: hydrochloric acid = 1:5:5), and then 2 L of Tris-HCl (pH = 9) solution was prepared, and the Tris-HCl solution was added to the acid-treated glass bottle. Then 100 g of dopamine (DA) was weighed and added to the Tris-HCl solution. After stirring and mixing for 10 hours, the glass bottle was washed with ethanol and water for 5 times respectively until the ethanol or water after washing was transparent, and then placed in a 100°C oven for drying for 15 hours to obtain a glass bottle with a black polydopamine grafted on the inner surface; (2) Prepare 2L of 15mol / L concentrated hydrochloric acid, add 100g of nano-titanium dioxide particles, react in an oil bath at 130°C for 6h, then wash with ethanol and water repeatedly for 5 times, dry in an oven at 100°C for 15h to activate the surface of the nano-titanium dioxide particles, then prepare 2L of ethanol aqueous solution (ethanol and water are mixed in a volume ratio of 10:1), and drop 25 drops of silane coupling agent into the ethanol aqueous solution to activate the surface of the nano-titanium dioxide particles. Stir for 8min at 50°C to hydrolyze. After the reaction is completed, add 100g of surface-activated nano-titanium dioxide particles to the hydrolyzate and stir for 6h. Wash with ethanol and water for 3 times respectively, and dry in an oven at 100°C for 15h to obtain nano-titanium dioxide particles grafted with silane coupling agent; (3) Add 1 L of dilute hydrochloric acid with a pH of 6 into the glass bottle with the inner surface grafted with black polydopamine obtained in step (1), and then add 30 g of nano-titanium dioxide particles grafted with a silane coupling agent, stir at 50° C. for 15 h to allow an electrostatic transfer reaction to occur, wash with ethanol and water three times respectively, and dry in an oven at 100° C. for 15 h to obtain a black glass bottle with nano-titanium dioxide particles deposited on the surface.

[0023] According to the methods of implementation 1 to 3, the temperature resistance, acid resistance and alkali resistance test were carried out according to the hundred grid method test. The experimental results are shown in Table 1. The acidified glass was subjected to SEM test. Figure 1 SEM tests were performed on uncoated glass and treated glass bottles, as shown in Figures 1 to 4 , and the transmittance test was also carried out, such as Figure 5 .

Claims

1. A method for preparing a brown glass bottle for storing glue, characterized in that The steps include: (1) The inner surface of the glass bottle is treated with an acid, and then a Tris-HCl solution with a pH of 8 to 9 is prepared, and the Tris-HCl solution is added to the acid-treated glass bottle, and then dopamine is weighed and added to the Tris-HCl solution, and the amount of dopamine added is controlled to be 50 to 100 g, and the mixture is stirred and mixed to react, and after the reaction, the mixture is washed and dried to obtain a glass bottle with a black polydopamine grafted on the inner surface; (2) Activating the surface of the nano-inorganic particles, and then preparing an ethanol aqueous solution, and adding a silane coupling agent to the ethanol aqueous solution for hydrolysis reaction, controlling the amount of the silane coupling agent added to be 20-30 drops, adding the surface-activated nano-inorganic particles to the hydrolyzate after the reaction is completed, stirring, controlling the amount of the surface-activated nano-inorganic particles added to be 50-100 g, washing, and drying to obtain nano-inorganic particles grafted with a silane coupling agent; (3) In the glass bottle with the black polydopamine grafted on the inner surface obtained in step (1), an acid / base solution with a pH value greater than 4 is prepared, and nano-inorganic particles grafted with a silane coupling agent are added thereto, wherein the amount of the nano-inorganic particles grafted with a silane coupling agent is controlled to be 10-50 g, an electrostatic transfer reaction is caused by stirring, and 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 glue according to claim 1, characterized in that: The acid used for the acid treatment of the glass bottle in step (1) is a mixed acid, which is a mixture of hydrofluoric acid: concentrated sulfuric acid: hydrochloric acid in a volume ratio of 1: (2-5): (2-5).

3. The method for preparing a brown glass bottle for storing glue 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 glue according to claim 1, characterized in that: The method for surface activation of the nano inorganic particles in step (2) is: prepare 10-15 mol / L concentrated hydrochloric acid or 3-10 mol / L sodium hydroxide, add 20-300 g of silicon dioxide, titanium dioxide or hexagonal boron nitride, react in an oil bath at 100-200° C. for 5-10 hours, then wash repeatedly with ethanol and water for 2-5 times, and dry in an oven at 80-100° C.

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

1.

6. The method for preparing a brown glass bottle for storing glue according to claim 1, characterized in that: In the step (2), the silane coupling agent is one of kh550, kh570 and DC5700.

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

8. The method for preparing a brown glass bottle for storing glue according to claim 1, characterized in that: The stirring conditions in step (3) are 10-24 hours and 40-60°C.

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

10. A method for preparing a brown glass bottle for storing glue according to any one of claims 1 to 9, characterized in that: The drying conditions in step (1), step (2) and step (3) are: drying at 50-100°C.

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