A barrier film for large infusion soft bags

Abstract

The present invention relates to the field of infusion packaging, and more specifically to a barrier film for large infusion soft bags and a preparation method thereof. The film has a seven-layer structure, comprising, from the inside out, a heat seal layer, a first adhesive layer, a weather-resistant layer, a second adhesive layer, a barrier layer, a third adhesive layer, and a printed layer. The heat seal layer is composed of ethylene-propylene copolymer and SEBS, the first, second, and third adhesive layers are all composed of adhesive resins, the weather-resistant layer is composed of ethylene-octene copolymer, the barrier layer is composed of EVOH, and the printed layer is composed of polypropylene and SEBS. The film can effectively block gases such as water vapor, nitrogen, oxygen, and carbon dioxide, and can meet the various performance and requirements required for large infusion soft bags, reducing the complexity of pharmaceutical factory processes and the costs of pharmaceutical factories.

Description

Technical Field

[0001] The present invention relates to the field of infusion packaging, and in particular to a barrier film for a large infusion soft bag and a preparation method thereof. Technical Background

[0002] With the development and progress of science, pharmaceutical packaging materials are also undergoing significant changes. The packaging material for large-volume parenteral drugs has shifted from glass bottles to polyethylene and polypropylene. The packaging format has also gradually evolved from the original bottle type to a combination of bottle and bag types. Among them, non-PVC multi-layer co-extruded infusion bags are a very common packaging format for large-volume parenteral drugs on the market.

[0003] Non-PVC soft bags are multi-layer co-extruded infusion bags with excellent mechanical properties and stable physical and chemical properties. They are easy to transport and widely favored in the market. However, the multi-layer co-extruded infusion film currently used in China has poor moisture and gas barrier properties. High-barrier outer bags are generally used over the infusion soft bags, which increases process complexity and costs for pharmaceutical manufacturers. Summary of the Invention

[0004] The purpose of the present invention is to address the deficiencies of the above-mentioned prior art and provide a barrier film that can be used for large infusion soft bags. The barrier properties of this film are significantly superior to those of existing multi-layer co-extruded infusion films. It can effectively block gases such as water vapor, nitrogen, oxygen, and carbon dioxide, and can meet the various performance and requirements required for large infusion soft bags.

[0005] To achieve the above object, the technical solution of the present invention is as follows:

[0006] The present invention provides a barrier film that can be used in a large infusion soft bag. The film has a seven-layer structure, which includes, from the inside to the outside, a heat-sealing layer, a first adhesive layer, a weather-resistant layer, a second adhesive layer, a barrier layer, a third adhesive layer, and a printing layer.

[0007] The heat seal layer is composed of ethylene-propylene copolymer and SEBS, wherein the ethylene-propylene copolymer accounts for 80-90 parts and the SEBS accounts for 10-20 parts;

[0008] The first, second and third adhesive layers are all composed of adhesive resin, and the adhesive resin accounts for 100 parts;

[0009] The weather-resistant layer is composed of ethylene-octene copolymer, and the ethylene-octene copolymer accounts for 100 parts;

[0010] The barrier layer is composed of EVOH, with EVOH accounting for 100 parts;

[0011] The printing layer is composed of polypropylene and SEBS, with polypropylene accounting for 85-90 parts and SEBS accounting for 10-15 parts.

[0012] The total thickness of the barrier film is 190-250 μm, of which the heat sealing layer is 20-35 μm thick, the first, second and third adhesive layers are 5-10 μm thick, the weather-resistant layer is 120-150 μm thick, and the printing layer is 15-25 μm thick.

[0013] The density of the ethylene-propylene copolymer is 0.88-0.92 g / cm 3 , melt index is 5-7g / 10min, melting point is 110-130℃; density of SEBS is 0.88-0.91g / cm 3 , the melting point is 50-90℃, the melting index is 1-3g / 10min, the density of the adhesive resin is 0.86-0.92g / cm 3 , melt index is 0.5-3g / 10min, melting point is 55-90℃; EVOH has a density of 1-1.2g / cm3, a melt index of 3-5g / 10min, and a melting point of 150-190℃; the density of polypropylene is 0.88-0.9g / cm 3 , the melting index is 5-8g / 10min, and the melting point is 160-180℃.

[0014] The process for preparing a barrier film for a large infusion soft bag described in the present invention comprises the following steps:

[0015] (1) The present invention adopts a seven-layer co-extrusion downward-blowing water-cooled film blowing unit for processing, and the first step is to heat and keep the extruder die head warm;

[0016] (2) In the second step, the raw materials are mixed according to the formula requirements and pumped into the barrel of the corresponding extruder. After the temperature reaches a certain level, the raw materials are melted and extruded, blown down to form film bubbles, and then passed through a water ring cooling system, dried in a drying system, and rolled into a tube film.

[0017] (3) In the third step, the tube film is irradiated with electron beams and then cut into pieces to obtain a high-barrier film for infusion soft bags.

[0018] Step (1) is heated according to the heating step, with the heating temperature set at 180°C and then kept warm for 2 hours. The temperature is then set according to the characteristics of the materials of each layer, with the heat sealing layer temperature set at 200-220°C, the first, second, and third adhesive layers temperature set at 200-220°C, the weathering layer temperature set at 190-215°C, the barrier layer temperature set at 200-230°C, the printing layer temperature set at 200-230°C, and the die head temperature set at 210-240°C. Melting is performed at the corresponding temperatures, and the next step is performed after the temperatures are reached.

[0019] In step 2 (2), the water circulation flow rate is set to 24000-2600 L / h, the purified water temperature for cold cutting is set to 15-35°C, and the extrusion volume is set to 200-400 kg / h.

[0020] In step (3), the electron beam irradiation has a beam current of 40-45 mA, a high voltage of 0.48-0.52 MeV, and a linear speed of 7-10 m / min.

[0021] The production of the present invention is completed in a clean area. Compared with the existing technology, the present invention has the following advantages:

[0022] (1) Compared with traditional multi-layer co-extruded films, this product has absolute advantages in barrier properties and can meet the needs of almost all types of liquid medicines in pharmaceutical factories;

[0023] (2) Reduce process complexity and production costs of pharmaceutical factories;

[0024] (3) The weather-resistant layer is sterilized with ethylene, which gives it good mechanical properties and is superior to general barrier films in terms of impact resistance, tear resistance and high temperature resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic diagram of the seven-layer co-extruded film structure of a barrier film that can be used for large infusion soft bags. From top to bottom, it is the heat seal layer a, the first adhesive layer b, the weather-resistant layer c, the second adhesive layer d, the barrier layer e, the third adhesive layer f, and the printing layer g. DETAILED DESCRIPTION

[0026] The preferred embodiments of the present invention are described below. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0027] Polyethylene and polypropylene have excellent biosafety and drug compatibility, and multilayer co-extruded films made from them exhibit excellent weather resistance and drop resistance. However, their water and gas barrier properties are relatively poor, making them suitable only for standard infusion solutions. The present invention combines the advantages of existing multilayer co-extruded infusion films with the addition of a barrier layer, significantly improving their water and gas barrier properties and meeting the requirements of high-end infusion solutions in China.

[0028] The heat-seal layer is made of ethylene-propylene copolymer and SEBS. As the inner layer, ethylene-propylene copolymer offers excellent biosafety and drug compatibility, excellent heat-sealing properties, and resistance to external impact. The addition of SEBS increases the film's flexibility and lowers the unsealing temperature. The inner layer is bonded to the weather-resistant layer via an adhesive resin. The weather-resistant layer is made of ethylene-octene copolymer, which provides a certain degree of moisture barrier and flexibility, while also improving the film's low-temperature resistance. The weather-resistant layer is bonded to the barrier layer via an adhesive resin. EVOH is used as the barrier layer, providing excellent moisture barrier properties. The barrier layer is bonded to the printing layer via an adhesive resin. Polypropylene and SEBS are used for the printing layer. Polypropylene offers excellent heat-sealing properties, protection, and good printing performance. The addition of SEBS increases the film's flexibility.

[0029] The raw material manufacturers and models used in the following examples are as follows:

[0030] The ethylene-propylene copolymer was WFX4M from Polychem, Japan;

[0031] SEBS are G1645 from Kraton (USA) and H1062 and H1221 from Asahi Kasei (Japan);

[0032] The adhesive resins are Dow's 8150 and Mitsui Chemicals' NF529.

[0033] EVOH is H171B from Kuraray Co., Ltd. of Japan;

[0034] Polypropylene was FP570M from Basel;

[0035] The polyesters are ED004 and 9967 produced by Eastman Company.

[0036] Example 1

[0037] The total thickness of the film is 200μm, with the following thicknesses from top to bottom: 20μm, 10μm, 120μm, 10μm, 10μm, 10μm, and 20μm. The heat-seal layer is the inner layer and is composed of the following components and materials: 80 parts WFX4M and 20 parts G1645. Adjacent to the heat-seal layer is the first adhesive layer, composed of 100 parts 8150; followed by a weathering layer, composed of 100 parts 2010MA; followed by a second adhesive layer, composed of 100 parts NF529; a barrier layer, composed of 100 parts H171B; and a third adhesive layer, composed of 100 parts NF529. The final printing layer is composed of 85 parts FP570M, 7.5 parts H1221, and 7.5 parts H1062.

[0038] The large infusion soft bag can be prepared using a barrier film preparation method according to the following steps:

[0039] (1) Heat the extruder to 180°C and keep it warm for two hours. Then set the heat seal layer temperature to 218°C, the first adhesive layer temperature to 220°C, the weathering layer temperature to 215°C, the second adhesive layer temperature to 220°C, the barrier layer temperature to 220°C, the third adhesive layer temperature to 220°C, the printing layer temperature to 230°C, and the die head temperature to 220°C. Once the temperatures are reached, proceed to the next step.

[0040] (2) The water flow rate of the water ring is set to 2500L / h, the temperature of the purified water for cold cutting is set to 25℃, the extrusion volume is set to 300kg / h, and the product is basically rolled.

[0041] (3) The beam current is set to 45 mA, the high voltage is set to 0.5 MeV, and the line speed is controlled at 7.5 m / min. The film material is irradiated with electron beam and then cut.

[0042] Example 2

[0043] The total thickness of the film is 200μm, with the following thicknesses from top to bottom: 30μm, 10μm, 125μm, 10μm, and 25μm. The heat-seal layer is the inner layer and is composed of the following components and materials: 80 parts WFX4M and 20 parts G1645. Adjacent to the heat-seal layer is the first adhesive layer, composed of 100 parts 8150. Next is the weathering layer, composed of 100 parts 2010MA. Following this is the second adhesive layer, composed of 100 parts 8150. Finally, the printed layer is composed of 60 parts 9967 and 40 parts ED004.

[0044] Example 2 is a five-layer co-extruded infusion film, which is prepared according to the following steps:

[0045] (1) Heat the extruder to 180°C and keep it warm for two hours. Then set the heat seal layer temperature to 218°C, the first adhesive layer temperature to 220°C, the weathering layer temperature to 215°C, the second adhesive layer temperature to 220°C, the printing layer temperature to 230°C, and the die head temperature to 230°C. Once the temperatures are reached, proceed to the next step.

[0046] (2) The water flow rate of the water ring is set to 2500L / h, the temperature of the purified water for cold cutting is set to 25℃, the extrusion volume is set to 300kg / h, and the product is basically rolled.

[0047] (3) The beam current is set to 45 mA, the high voltage is set to 0.5 MeV, and the line speed is controlled at 7.5 m / min. The film material is irradiated with electron beam and then cut.

[0048] Example 3

[0049] The total thickness of the membrane material is 120μm, all of which is a weather-resistant layer composed of 100 parts of 2010MA.

[0050] Example 3 Preparation method The preparation was carried out according to the following steps:

[0051] (1) Heat the extruder to 180°C and keep it warm for two hours. Set the weathering layer temperature to 215°C and the die head temperature to 220°C. Once the temperatures are reached, proceed to the next step.

[0052] (2) The water flow rate of the water ring is set to 2500L / h, the temperature of the purified water for cold cutting is set to 25℃, the extrusion volume is set to 300kg / h, and the product is basically rolled.

[0053] (3) The beam current is set to 45 mA, the high voltage is set to 0.5 MeV, and the line speed is controlled at 7.5 m / min. The film material is irradiated with electron beam and then cut.

[0054] Example 4

[0055] The total thickness of the membrane material is 120μm, all of which is a weather-resistant layer composed of 100 parts of 2010MA.

[0056] Example 4 Preparation method The preparation was carried out according to the following steps:

[0057] (1) Heat the extruder to 180°C and keep it warm for two hours. Set the weathering layer temperature to 215°C and the die head temperature to 220°C. Once the temperatures are reached, proceed to the next step.

[0058] (2) The water flow rate of the water ring is set to 2500L / h, the temperature of the purified water for cold cutting is set to 25℃, the extrusion volume is set to 300kg / h, and the product is basically rolled and then slit.

[0059] The membrane materials, Example 1 and Example 2, were tested according to the YBB00112005-2015 standard, and all items met the standard requirements. The water and gas barrier performance was compared, and the specific results are as follows:

[0060]

[0061] The high temperature boiling resistance test was carried out on the produced Example 3 and Example 4. The specific results are as follows:

[0062] project Example 3 Example 4 Can it withstand cooking at 121°C? yes no

[0063] The data demonstrates that the barrier film produced using this process meets the YBB requirements of pharmaceutical manufacturers and significantly outperforms five-layer, co-extruded infusion films in terms of water and gas barrier properties. This process also enhances the film's high-temperature resistance, meeting the pharmaceutical manufacturer's 121°C wet heat sterilization requirements.

[0064] The above is only one example of the invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A process for preparing a barrier film for a large infusion soft bag, characterized in that: The barrier film for large infusion soft bags is a seven-layer co-extruded infusion barrier film, which consists of a heat seal layer, a first adhesive layer, a weather resistant layer, a second adhesive layer, a barrier layer, a third adhesive layer, and a printing layer from the inside to the outside. The preparation process comprises the following steps: (1) A seven-layer co-extrusion bottom-blowing water-cooled film blowing unit is used for processing, and the extruder die head is heated and kept warm; (2) The raw materials are mixed according to the formula and pumped into the barrel of the corresponding extruder. After the temperature reaches the required level, the materials are melted and extruded, blown down to form film bubbles, and then passed through the water ring cooling system, dried in the drying system, and rolled into a tube film. The heat seal layer is composed of ethylene-propylene copolymer and SEBS; the ethylene-propylene copolymer is WFX4M from Polychem of Japan; The first, second and third adhesive layers are all made of adhesive resin; the adhesive resin is Dow's 8150 and Mitsui Chemicals' NF529. The weathering layer is composed of ethylene-octene copolymer; The barrier layer is composed of EVOH; EVOH is H171B from Kuraray Japan; The printing layer is composed of polypropylene and SEBS; the polypropylene is FP570M from Basel; SEBS are H1062 and H1221 from Asahi Kasei of Japan; The heat seal layer contains 80-90 parts of ethylene-propylene copolymer and 10-20 parts of SEBS; The adhesive resin in the first, second and third adhesive layers accounts for 100 parts; The weather-resistant layer contains 100 parts of ethylene-octene copolymer; The barrier layer contains 100 parts of EVOH; The printing layer contains 85-90 parts of polypropylene and 10-15 parts of SEBS; (3) The tube film is subjected to electron beam irradiation, with a beam current of 40-45 mA, a high voltage of 0.48-0.52 MeV, and a linear speed of 7-9 m / min. The tube film is then cut to obtain a high-barrier film for infusion soft bags.

2. The process for preparing the barrier film for large infusion soft bags according to claim 1, characterized in that: Step (1) is to heat according to the heating step, the heating temperature is set at 180°C, and then kept warm for 2 hours.

3. The process for preparing the barrier film for large infusion soft bags according to claim 1, characterized in that: In step (2), the temperature is set according to the material of each layer, the heat sealing layer temperature is set to 200-220°C, the first, second and third adhesive layers are set to 200-220°C, the weathering layer temperature is set to 190-215°C, the barrier layer temperature is set to 200-230°C, the printing layer temperature is set to 200-230°C, and the die head temperature is set to 210-240°C.

4. The process for preparing the barrier film for large infusion soft bags according to claim 1, characterized in that: The total thickness of the barrier film is 190-250 μm, of which the heat sealing layer is 20-35 μm, the first, second and third adhesive layers are 5-10 μm, the weathering layer is 120-150 μm and the printing layer is 15-25 μm.

5. The process for preparing the barrier film for large infusion soft bags according to claim 1, characterized in that: The density of ethylene-propylene copolymer is 0.88-0.92 g / cm 3 , the melting index is 5-7g / 10min, and the melting point is 110-130℃; The density of SEBS is 0.88-0.91g / cm 3 , the melting point is 1-3g / 10min, and the melting point is 50-90℃; The density of the adhesive resin is 0.86-0.92g / cm 3 , the melting index is 0.5-3g / 10min, and the melting point is 55-90℃; The density of EVOH is 1-1.2g / cm 3 , the melting index is 3-5g / 10min, and the melting point is 150-190℃; The density of polypropylene is 0.88-0.9g / cm 3 , the melting index is 5-8g / 10min, and the melting point is 160-180℃.

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