Method for reducing content of alkali ions on inner surface of glass storage bottle

Abstract

The invention discloses a method for reducing the content of alkali ions on the inner surface of a glass storage bottle, and belongs to the technical field of glass material dealkalization. Compared with other methods for reducing the content of alkali ions on the inner surface of the glass storage bottle, ferrous sulfate is used for dealkalizing the glass storage bottle at high temperature; no pollution is caused to the environment; sulfur dioxide is not directly used, so that the damage to equipment is small; ferrous sulfate is slowly decomposed into sulfide gas, so that the content of alkali metal ions on the inner surface of the glass storage bottle can be uniformly reduced. After the cleaned glass storage bottle is treated by ferrous sulfate for 10-40 minutes at the temperature of 540-580 DEG C, the content of alkali metal ions on the inner surface of the glass storage bottle is reduced by 60% as high as that before dealkalization, so that the glass storage bottle can meet the requirement of strict control on metal ion precipitation when special liquid is contained.

Description

Technical Field

[0001] The invention relates to the technical field of dealkalization of glass materials, and in particular to a method for reducing the alkali ion content on the inner surface of a glass storage bottle. Background Art

[0002] Glass has excellent thermal stability, chemical stability, optical, mechanical and other properties, and is an excellent packaging and storage material. However, with the continuous application of glass storage materials, the performance of glass storage bottles can no longer meet the strict storage requirements of some high-end materials (such as photoresists, etc.) for gold impurity precipitation, particle size and other indicators, and the inner surface of glass storage bottles needs to be treated.

[0003] In order to improve the water resistance of the inner surface of glass storage bottles and control the precipitation of alkali metal ions on the inner surface of glass storage bottles, it is necessary to reduce the alkali metal ion content on the inner surface of glass storage bottles. At present, the main methods for reducing the alkali metal ion content on the inner surface of glass storage bottles include acid treatment and difluoroethane (DFE) treatment. The commonly used substances for acid treatment are sulfur dioxide (SO 2 ) and ammonium sulfate (NH 4 ) 2 SO 4 ), the former is easy to cause SO during production 2 The latter will emit a large amount of nitrogen-containing gas during the production process, affecting the ecology. Summary of the invention

[0004] The object of the present invention is to provide a method for reducing the alkali metal ion content on the inner surface of a glass storage bottle, which can achieve the purpose of "de-alkali" and does not cause pollution to the environment during production.

[0005] The gaseous product after the decomposition of ferrous sulfate is only sulfide gas. After the complete reaction, no gas will be discharged. The DSC test results of ferrous sulfate heptahydrate are as follows: Figure 1 The reaction is as follows:

[0006] FeSO 4 ·(H 2 O) 7 →FeSO 4 ·(H 2 O) 4 +3H 2 O

[0007] FeSO 4 ·(H 2 O) 4 →FeSO 4 ·(H 2 O)+3H 2 O

[0008] FeSO 4 ·(H 2 O)→FeSO 4 +H 2 O

[0009] FeSO 4 →0.5Fe 2 SO 3 +0.5SO 2 +0.5SO 3

[0010] The DSC results show that ferrous sulfate begins to slowly decompose and release sulfide gas at 540°C, and this temperature range is the same as the temperature range of sulfur dioxide dealkalization. The slow decomposition of ferrous sulfate to generate sulfide gas can evenly reduce the alkali metal ion content on the inner surface of the glass storage bottle.

[0011] The purpose of the present invention can be achieved through the following technical solutions:

[0012] A method for reducing the alkali ion content on the inner surface of a glass storage bottle comprises the following steps:

[0013] Step 1, cleaning and drying the inner surface of the glass storage bottle;

[0014] Step 2: Add ferrous sulfate into a glass storage bottle, seal the bottle mouth and dealkalize at high temperature;

[0015] Step three, adding the cooled glass bottle into deionized water for ultrasonic treatment to complete the dealkalization of the glass storage bottle.

[0016] As a further solution of the present invention: the ferrous sulfate added in step 2 is ferrous sulfate heptahydrate.

[0017] As a further solution of the present invention: the ferrous sulfate added in step 2 is contained in a quartz tube and does not directly contact with the glass storage bottle.

[0018] As a further solution of the present invention: the ferrous sulfate added in step 2 is 2% to 3% of the capacity of the glass storage bottle.

[0019] As a further solution of the present invention: the high temperature dealkalization method is: after sealing the mouth of the glass storage bottle, dealkalization is carried out at a temperature of 540° C. to 580° C.

[0020] As a further solution of the present invention: the dealkalization time is 10 to 40 minutes.

[0021] As a further solution of the present invention: the glass bottle is made of the following raw materials in percentage by mass: SiO 2 60-70%, Al 2 O 3 1-3%, B2 O 3 0.1-1%, Na 2 O 7-15%, K 2 O 0.1-1%, MgO1-5%, CaO 7-15%, BaO0.1%-1%, Fe 2 O 3 0.1-1%.

[0022] Beneficial effects of the present invention:

[0023] 1. The present invention uses ferrous sulfate to reduce the alkali metal ion content on the inner surface of the glass storage bottle, does not directly use sulfur dioxide and nitrogen-containing substances in the production process, and has little impact on the ecological environment.

[0024] 2. The present invention uses ferrous sulfate for dealkalization, which greatly reduces the percentage of alkali metal ion content on the inner surface of the glass bottle after dealkalization, and can meet the strict requirements of glass storage bottles for controlling the precipitation of metal ions.

[0025] 3. The present invention uses ferrous sulfate for dealkalization, which can evenly reduce the alkali metal ion content on the inner surface of the glass storage bottle. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The present invention will be further described below in conjunction with the accompanying drawings.

[0027] Figure 1 This is the DSC test diagram of ferrous sulfate heptahydrate. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] See also Figure 1 As shown, the specifications of the glass storage bottle used in the present invention are as follows: the capacity of the glass bottle is 4L, the diameter of the bottle mouth is 35mm, the height is 340mm, and the composition mass percentage is as follows: Si O 2 67%, A l 2 O 3 2%, B 2 O 3 0.5%, Na 2 O10%, K 2 O 1%, MgO 2.5%, CaO 10%, BaO 1%, Fe 2 O 3 1%.

[0030] Embodiment 1 of the present invention does not perform any processing.

[0031] Examples 2-5 of the present invention were prepared by the following method:

[0032] Use an electronic balance to weigh 2% to 4% of the capacity of the glass bottle of ferrous sulfate heptahydrate and put it into a quartz tube with a hole on the side, insert the quartz tube into the glass storage bottle and suspend it in the middle of the glass storage bottle, put the sealed glass bottle into a muffle furnace with a temperature of T0, 540℃≤T0≤580℃, and the dealkalization time is 10, 20, 30, and 40 minutes respectively.

[0033] After the glass storage bottle is cooled to room temperature, it is ultrasonically treated with deionized water for 30 minutes to clean off the solid products scattered on the bottom of the bottle and the alkali metal ion compounds such as sodium sulfate precipitated during the dealkalization process, and then dried for performance testing.

[0034] The shoulders, bodies and bottoms of the treated glass storage bottles were tested by X-ray energy dispersive spectrometer (EDS). The alkali metal ion content (in terms of Na 2 The results are shown in Table 1.

[0035] Table 1 Na2O content on the inner surface of each part after different treatment time

[0036]

[0037] As can be seen from Table 1, the alkali metal ion content on the inner surface of the treated glass storage bottle has decreased significantly. As the treatment time increases, the decrease in alkali metal ion content gradually increases. When the treatment time reaches 30 minutes, the decrease in alkali metal ion content is high. As the treatment time is extended, the decrease in alkali metal ion content decreases. According to EDS testing, when using ferrous sulfate to reduce the alkali metal ion content on the inner surface of the glass storage bottle, the optimal treatment time is 30 minutes.

[0038] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for reducing the alkali ion content on the inner surface of a glass storage bottle, characterized in that: The following steps are involved: Step 1, cleaning and drying the inner surface of the glass storage bottle; Step 2: Add ferrous sulfate into a glass storage bottle, seal the bottle mouth and dealkalize at high temperature; Step three, adding the cooled glass bottle into deionized water for ultrasonic treatment to complete the dealkalization of the glass storage bottle.

2. A method for reducing the alkali ion content on the inner surface of a glass storage bottle according to claim 1, characterized in that: The ferrous sulfate added in step 2 is ferrous sulfate heptahydrate.

3. A method for reducing the alkali ion content on the inner surface of a glass storage bottle according to claim 1, characterized in that: The ferrous sulfate added in step 2 is contained in a quartz tube and does not directly contact the glass storage bottle.

4. A method for reducing the alkali ion content on the inner surface of a glass storage bottle according to claim 1, characterized in that: The amount of ferrous sulfate added in step 2 is 2%-3% of the capacity of the glass storage bottle.

5. A method for reducing the alkali ion content on the inner surface of a glass storage bottle according to claim 4, characterized in that: The high temperature dealkalization method is: after sealing the mouth of the glass storage bottle, dealkalization is carried out at a temperature of 540°C-580°C.

6. A method for reducing the alkali ion content on the inner surface of a glass storage bottle according to claim 5, characterized in that: The dealkalization time is 10-40 minutes.

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