Preparation method of injection bottle made of ultrahigh-water-resistance neutral borosilicate glass tube

By adjusting the process parameters in the preparation method, the uniform heating of the glass tube and the stability of the alkali-boron phase are ensured, and the water resistance problem caused by uneven heating of the existing glass tube injection bottles is solved, and the uniformity of volatility and water resistance of the surface substances in the injection bottles are improved.

CN120192083APending Publication Date: 2025-06-24GERRESHEIMER SHUANGFENG PHARM GLASS DANYANG CO LTD
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Patent Information

Application Number
CN202510336184.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-20
Publication Date
2025-06-24

AI Technical Summary

Technical Problem

When the existing glass tube injection bottles are unevenly heated, the alkali boron phase substances will be volatile in different degrees, which will affect the water resistance of the injection bottles.

Method used

By adjusting the process parameters in the preparation method, including adjusting the speed, annealing temperature and blowing pressure of the bottle making machine according to the injection bottle of different specifications, ensuring uniform heating of the glass tube and the stability of the alkali-boron phase.

Benefits of technology

The uniformity of volatility of the substances in the inner surface of the injection bottle is achieved, the water resistance of the injection bottle is improved, and the problem of decreasing water resistance caused by uneven heat is avoided.

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Abstract

The invention belongs to the technical field of glass bottle processing, and particularly relates to a preparation method of an injection bottle made of a neutral borosilicate glass tube with ultrahigh water resistance, which comprises the following steps: (1) raw material selection and inspection: selecting a neutral borosilicate glass tube with water resistance, and inspecting the size, appearance and physicochemical properties of the neutral borosilicate glass tube; (2) making a bottle: placing the glass tube on a bottle making machine, supplying gas and heating to a softening point, and sequentially pressing a bottle head and a bottle bottom into an injection bottle by using a mold; and (3) annealing: placing the pressed injection bottle in an annealing furnace for annealing. The machine speed, the annealing temperature and the blowing pressure of the bottle making machine are adjusted according to injection bottles of different specifications, the glass tube can be better and evenly heated, the glass tube can be evenly heated, volatilization of an alkali boron phase can be controlled, and the water resistance of the prepared injection bottles cannot be affected.
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Description

Technical Field

[0001] The present invention belongs to the technical field of glass bottle processing, and particularly relates to a preparation method of a neutral borosilicate glass tube injection bottle with ultra-high water resistance. Background Art

[0002] Drugs are special commodities. As pharmaceutical glass used as packaging materials, it has to be in direct contact with drugs, and most of them also need to store drugs for a long time. Therefore, some components in the glass may be dissolved by the drugs in contact or cause mutual migration of components, and may also be eroded by the liquid medicine for a long time to cause delamination, which directly affects the quality of drugs or the dosage. Due to the wide variety of drugs and complex active genes, for example, for strong alkaline drugs filled in ampoules, some components may be dissolved or glass delamination may occur, and glass delamination is a potential hazard for thrombosis formation. Therefore, the performance and quality of pharmaceutical glass directly affect the quality of drugs and are closely related to people's health and safety.

[0003] A borosilicate glass tube injection bottle is an injection bottle made of neutral borosilicate glass. Neutral borosilicate glass is the so-called type I glass, and some in China also call it 5.0 glass or grade A material. This type of glass has been widely used in the field of drug packaging due to its good material and performance, especially its excellent chemical stability and thermal stability.

[0004] At present, imported formed glass tubes are mostly selected for secondary forming processing in the production of glass tube injection bottles. However, due to the different sealing methods of the two ends of the glass tubes by each glass tube supplier, it is easy to cause uneven heating inside and outside the glass tube during secondary processing, and then cause different volatilization degrees of the volatile components of the glass tube, affecting the water resistance of the prepared injection bottle. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method of a neutral borosilicate glass tube injection bottle with ultra-high water resistance to solve the problem that uneven heating affects the water resistance of the injection bottle in the prior art during the production of glass tube injection bottles. There is no problem of uneven volatilization of substances on the inner surface of the injection bottle prepared by this method, which affects the water resistance of the injection bottle.

[0006] The specific technical solution is as follows:

[0007] A preparation method of a neutral borosilicate glass tube injection bottle with ultra-high water resistance, characterized by comprising the following steps:

[0008] (1) Raw material selection and inspection: Select a neutral borosilicate glass tube with water resistance, and inspect its size, appearance and physical and chemical properties;

[0009] (2) Bottle making: Place the glass tube on the bottle making machine, supply gas and heat it to the softening point, and use the mold to press the bottle head and the bottle bottom into an injection bottle in sequence;

[0010] (3) Annealing: Place the pressed injection bottle in an annealing furnace for annealing.

[0011] Furthermore, the pipe diameter sizes of the glass tube in step (1) include the following specifications: 16 mm and below, greater than 16 mm and less than or equal to 18.4 mm, greater than 18.4 mm and less than or equal to 22 mm, greater than 22 mm and less than or equal to 27.5 mm, greater than 27.5 mm and less than or equal to 30 mm.

[0012] Furthermore, the following steps are included in step (2): Place the glass tube on the bottle making machine, set a fixture on the bottle making machine, set a cam mechanism at the bottom of the fixture, the bottom of the fixture is in transmission connection with the cam, and a high-temperature heating gas injection pipe, an auxiliary gas heating injection pipe, and a compressed air injection pipe are arranged on the side of the fixture; the fixture clamps the glass tube and passes through a preheating lamp head, a punching lamp head, and a cutting lamp head in sequence for heating, cutting and pulling the material, and making the bottle.

[0013] Furthermore, the machine speed of the bottle making machine in step (2) is set as follows: the machine speed for a pipe diameter of 16 mm and below is 20 - 21 strokes / min, the machine speed for a pipe diameter greater than 16 mm and less than or equal to 18.4 mm is 21 - 22 strokes / min, the machine speed for a pipe diameter greater than 18.4 mm and less than or equal to 22 mm is 19 - 21 strokes / min, the machine speed for a pipe diameter greater than 22 mm and less than or equal to 27.5 mm is 18 - 20 strokes / min, and the machine speed for a pipe diameter greater than 27.5 mm and less than or equal to 30 mm is 17 - 19 strokes / min.

[0014] Furthermore, the number of times of adding the hydrolysis solution in step (3) is 2 - 6 times, preferably 3 - 5 times; the interval time between each addition is 10 - 40 min, preferably 20 - 30 min; the reaction temperature is 20 - 60 °C, preferably 20 - 40 °C; stirring is maintained during the feeding and continuous reaction process, the stirring speed is 500 - 600 rpm, and the continuous reaction time is 1 - 2 h.

[0015] Furthermore, the cam in step (2) is irregular in shape, and the cam includes continuous circular regions, convex regions, and concave regions.

[0016] Furthermore, the pressure of the high-temperature heating gas injection pipe in step (2) is 0.02 - 0.03 MPa, and the pressure of the auxiliary gas heating injection pipe is 0.03 - 0.05 MPa; the compressed air injection pipe is provided with low-pressure air and high-pressure air, the pressure of the low-pressure air is 0.02 - 0.04 Mpa, and the pressure of the high-pressure air is 0.6 - 0.7 MPa.

[0017] Further, in the step (3), the annealing temperature is set as follows: for a tube diameter of 16 mm or less, the annealing temperature is 570 - 580 °C; for a tube diameter greater than 16 mm and less than or equal to 18.4 mm, the annealing temperature is 580 - 590 °C; for a tube diameter greater than 18.4 mm and less than or equal to 22 mm, the annealing temperature is 580 - 600 °C; for a tube diameter greater than 22 mm and less than or equal to 27.5 mm, the annealing temperature is 590 - 610 °C; for a tube diameter greater than 27.5 mm and less than or equal to 30 mm, the annealing temperature is 600 - 620 °C.

[0018] Beneficial effects:

[0019] In view of the problem that in the production of existing glass - controlled injection vials, the alkali - boron phase substances will have different volatilization degrees due to uneven heating, resulting in a decrease in the water resistance of the inner surface of the prepared injection vials, by adjusting the process parameters in the preparation method, especially adjusting the machine speed, annealing temperature, and blowing pressure of the bottle - making machine according to different specifications of injection vials, the glass tube can be heated more evenly, so that it is heated uniformly and the volatilization of the alkali - boron phase can be controlled, without affecting the water resistance of the prepared injection vials. Description of the drawings

[0020] Figure 1 It is the top view of the cam in the present invention;

[0021] Figure 2 It is the annealing curve graph of the embodiment in the present invention. Detailed implementation manners

[0022] The following further elaborates on the technical solutions of the present invention with specific embodiments, but the protection scope of the present invention is not limited to the following embodiments.

[0023] Embodiment

[0024] This embodiment provides a preparation method for a neutral borosilicate glass - controlled injection vial with ultra - high water resistance, including the following steps:

[0025] (1) Raw material selection and inspection: Select a neutral borosilicate glass tube with water resistance, and inspect its size, appearance, and physical and chemical properties;

[0026] Specifically, select a neutral borosilicate glass tube with water resistance, such as the neutral borosilicate glass tube produced by Schott or Corning. Inspect that the water resistance of the glass tube meets the standard. After passing the inspection, classify and reserve it according to the tube diameter size. The tube diameter sizes are divided into 16 mm and below, greater than 16 mm and less than or equal to 18.4 mm, greater than 18.4 mm and less than or equal to 22 mm, greater than 22 mm and less than or equal to 27.5 mm, and greater than 27.5 mm and less than or equal to 30 mm.

[0027] (2) Bottle making: Place the glass tube on the bottle making machine, supply gas and heat it to the softening point, and use a mold to press the bottle head and the bottle bottom into an injection bottle in sequence;

[0028] Specifically, place the glass tube on the bottle making machine. A fixture is set on the bottle making machine, and the glass bottle is clamped on the fixture with the bottle mouth facing down and the bottle bottom facing up. A cam mechanism is set at the bottom of the fixture, and the bottom of the fixture is in transmission connection with the cam. The cam mechanism is specifically as shown in the appendix Figure 1 As shown, it adopts an irregular style, including a circular area 1, a convex area 2 and a concave area 3. In this way, when the cam moves, it drives the glass bottle to pass through the cutting lamp head, and it is not directly cut, reducing the gas consumption of the cutting lamp head.

[0029] The machine speed of the bottle making machine is set according to the product pipe diameter size, specifically as follows: when the pipe diameter is 16 mm and below, the machine speed is 20 - 21 strokes / min; when the pipe diameter is greater than 16 mm and less than or equal to 18.4 mm, the machine speed is 21 - 22 strokes / min; when the pipe diameter is greater than 18.4 mm and less than or equal to 22 mm, the machine speed is 19 - 21 strokes / min; when the pipe diameter is greater than 22 mm and less than or equal to 27.5 mm, the machine speed is 18 - 20 strokes / min; when the pipe diameter is greater than 27.5 mm and less than or equal to 30 mm, the machine speed is 17 - 19 strokes / min.

[0030] A high-temperature heating gas injection pipe, an auxiliary gas heating injection pipe and a compressed air injection pipe are set on the side of the fixture. The glass bottle is placed on the fixture, and high-temperature heating is carried out by aligning the heating gas and the auxiliary gas with a distance of 3.5 - 7 mm from the bottle bottom or the bottle mouth of the glass bottle. The heating gas is natural gas, and the auxiliary gas is oxygen. Natural gas is the main heating gas, and oxygen is used as an auxiliary. Oxygen can improve the combustion efficiency of acetylene or natural gas and increase the flame temperature. The heating temperature is 1500 - 1600 °C. When burning, the pressure of natural gas is 0.02 - 0.03 MPa, and the pressure of oxygen is 0.03 - 0.05 MPa. The compressed air injection pipe is provided with low-pressure air and high-pressure air. The pressure of low-pressure air: 0.02 - 0.04 Mpa, and the pressure of high-pressure air: 0.6 - 0.7 MPa.

[0031] In this application, a multi-station forming technology is adopted. The bottle making machine rotates around the axis, and the glass tube is clamped and passes through the preheating lamp head, the punching lamp head and the cutting lamp head in sequence for heating, cutting and pulling materials and bottle making.

[0032] Under the preheating lamp head, heating starts at a horizontal distance of 7 mm from the bottom surface of the glass tube. During the heating process, the cam drives the glass bottle to rotate at a constant speed. The rotation speed of the cam during the heating process of the glass bottle is 1 r / s.

[0033] After the glass tube is preheated at the punching lamp head, the punching lamp head is 5 mm away from the bottom surface of the glass tube, and the flame of the punching lamp head vertically penetrates through the center of the glass tube. In this way, the glass tube is not easily unevenly heated during the heating process, which may cause different volatilization degrees of the alkali-boron phase in the glass tube and affect the water resistance of the inner surface of the glass bottle.

[0034] After being heated by the punching lamp head, the glass tube is heated to soften and enters the cutting and drawing lamp head. When processing glass tubes with a diameter of less than 22 mm, the cutting and drawing lamp head uses a 13-hole 0.7-mm lamp head, and the horizontal position is 3.5 mm away from the cut glass tube. When processing glass tubes with a diameter greater than 22 mm and less than or equal to 27.5 mm, a 15-hole 0.7-mm lamp head is used, and the horizontal position is 5 mm away from the cut glass tube. When processing glass tubes with a diameter greater than 27.5 mm, a 19-hole 0.7-mm lamp head is used, and the horizontal position is 5 mm away from the cut glass tube. After cutting and drawing, a mold is used to first form the bottle head of the glass tube and then form the bottle bottom to make an injection bottle of the corresponding specification.

[0035] During the heating process of the bottle making machine, an intermittent blowing device is also provided to control the shape of the glass bottle and remove the volatile white mist generated by heating. At the preheating lamp head, the blowing device blows air into the glass tube, and the blowing pressure is 0.2 MPa. The intermittent time of the intermittent blowing device is 0.5 beats / min.

[0036] (3) Annealing: Place the pressed injection bottle in an annealing furnace for annealing.

[0037] Specifically, anneal the made injection bottle in the annealing furnace, and the annealing temperature is determined according to the specification of the injection bottle. For glass tubes with a diameter of 16 mm and below, the annealing temperature is 570 - 580 °C; for glass tubes with a diameter greater than 16 mm and less than or equal to 18.4 mm, the annealing temperature is 580 - 590 °C; for glass tubes with a diameter greater than 18.4 mm and less than or equal to 22 mm, the annealing temperature is 580 - 600 °C; for glass tubes with a diameter greater than 22 mm and less than or equal to 27.5 mm, the annealing temperature is 590 - 610 °C; for glass tubes with a diameter greater than 27.5 mm and less than or equal to 30 mm, the annealing temperature is 600 - 620 °C. The annealing temperature curve is as shown in the appendix Figure 2 shown. After annealing, place the injection bottle in a continuous slow cooling kiln for cooling, and the cooled temperature is 50 °C.

[0038] Unless otherwise specified, the terms used in the present invention have the meanings commonly understood by those skilled in the art. The embodiments described in the present invention are only for illustrative purposes and are not intended to limit the protection scope of the present invention. Those skilled in the art can make various other substitutions, changes, and improvements within the scope of the present invention. Therefore, the present invention is not limited to the above embodiments, but is only defined by the claims.

Claims

1. A method for preparing an ultra-high water-resistant neutral borosilicate glass tube injection bottle, characterized in that: The following steps are involved: (1) Raw material selection and inspection: Select neutral borosilicate glass tubes with water resistance and inspect their size, appearance, and physical and chemical properties; (2) Bottle making: Place the glass tube on a bottle making machine, heat it to the softening point with air supply, and use a mold to press the bottle head and bottle bottom in sequence to form an injection bottle; (3) Annealing: The pressed injection bottle is placed in an annealing furnace for annealing.

2. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 1, characterized in that: The diameter of the glass tube in step (1) includes the following specifications: 16 mm and below, greater than 16 mm and less than or equal to 18.4 mm, greater than 18.4 mm and less than or equal to 22 mm, greater than 22 mm and less than or equal to 27.5 mm, and greater than 27.5 mm and less than or equal to 30 mm.

3. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 1, characterized in that: The step (2) comprises the following steps: placing the glass tube on a bottle making machine, arranging a clamp on the bottle making machine, arranging a cam mechanism at the bottom of the clamp, the bottom of the clamp is connected to the cam by transmission, and arranging a high-temperature heating gas injection pipe, an auxiliary gas heating injection pipe and a compressed air injection pipe on the side of the clamp; the clamp clamps the glass tube and passes it through a preheating lamp head, a punching lamp head, a cutting lamp head in sequence to perform heating, cutting, drawing and bottle making.

4. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 3, characterized in that: In step (2), the machine speed of the bottle making machine is set as follows: the machine speed for tubes with a diameter of 16 mm or less is 20 to 21 beats / min, the machine speed for tubes with a diameter greater than 16 mm and less than or equal to 18.4 mm is 21 to 22 beats / min, the machine speed for tubes with a diameter greater than 18.4 mm and less than or equal to 22 mm is 19 to 21 beats / min, the machine speed for tubes with a diameter greater than 22 mm and less than or equal to 27.5 mm is 18 to 20 beats / min, and the machine speed for tubes with a diameter greater than 27.5 mm and less than or equal to 30 mm is 17 to 19 beats / min.

5. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 3, characterized in that: In the step (2), the cam is irregular in shape, and includes continuous circular areas, convex areas and concave areas.

6. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 3, characterized in that: In the step (2), the pressure of the high-temperature heating gas injection pipe is 0.02-0.03MPa, and the pressure of the auxiliary gas heating injection pipe is 0.03-0.05MPa; the compressed air injection pipe is provided with low-pressure wind and high-pressure wind, the low-pressure wind pressure is 0.02-0.04Mpa, and the high-pressure wind pressure is 0.6-0.7MPa.

7. The method for preparing a neutral borosilicate glass tube injection bottle with ultra-high water resistance according to claim 1, characterized in that: The annealing temperature in the step (3) is set as follows: the annealing temperature for a tube diameter of 16 mm or less is 570-580° C., the annealing temperature for a tube diameter greater than 16 mm and less than or equal to 18.4 mm is 580-590° C., the annealing temperature for a tube diameter greater than 18.4 mm and less than or equal to 22 mm is 580-600° C., the annealing temperature for a tube diameter greater than 22 mm and less than or equal to 27.5 mm is 590-610° C., and the annealing temperature for a tube diameter greater than 27.5 mm and less than or equal to 30 mm is 600-620° C.