CN113736176B - Composite food-grade oral liquid bottle and preparation method thereof - Google Patents
Composite food-grade oral liquid bottle and preparation method thereof Download PDFInfo
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- CN113736176B CN113736176B CN202111076080.5A CN202111076080A CN113736176B CN 113736176 B CN113736176 B CN 113736176B CN 202111076080 A CN202111076080 A CN 202111076080A CN 113736176 B CN113736176 B CN 113736176B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/10—Applications used for bottles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention discloses a composite food-grade oral liquid bottle and a preparation method thereof. The composite food-grade oral liquid bottle comprises the following compound components: 70-90 parts of food-grade polypropylene resin, 5-15 parts of food-grade high-density polyethylene, 5-15 parts of food-grade polyphenylene sulfone and 0.5-1.0 part of modified color master batch. The invention prepares the high-strength oral liquid bottle with good acid resistance, alkali resistance and heat resistance through compounding specific raw materials, is not only beneficial to the storage stability of the oral liquid dosage forms of medicines and health-care foods, but also solves the quality risk of broken glass residues caused by using the glass bottle, does not need cleaning and drying procedures under clean condition production conditions, greatly reduces the production cost, and has good application prospect in the field of liquid preparation packaging.
Description
Technical Field
The invention relates to the field of liquid packaging containers for directly contacting with food and medicine oral liquid dosage forms, in particular to a composite food-grade oral liquid bottle and a preparation method thereof.
Background
The oral liquid bottle is a packaging container for containing liquid oral liquid medicines and health products. The preparation method of sterilizing after filling and sealing is adopted for producing oral liquid medicine and health care products, and the common high pressure steam sterilization conditions are 115 ℃, 30min or 121 ℃ and 20min, and the oral liquid bottle must have good heat resistance, corrosion resistance, high strength and water vapor permeability. Therefore, the prior oral liquid package basically uses glass bottles, and glass residues which are easy to break after being impacted with equipment in the production process of glass bottles cause potential safety hazards to consumers. In addition, cleaning, drying and disinfection treatment are needed before filling, so that the production cost is increased. The glass bottle is easy to break and leak in the process of carrying and transporting, causes product pollution and economic loss, has large weight and high transportation cost, and is inconvenient for consumers to carry about.
The plastic bottle package is not easy to be broken, has light weight, can be directly filled in the plastic bottle produced in a clean environment, can save procedures and cost, but has the problem of low heat resistance and easy deformation of common plastics.
For example, CN109749232a discloses a preparation method of an oral liquid plastic bottle: mixing plastic particles with a nucleating agent in proportion, and then blending and modifying the mixture by a double-screw extruder to obtain a polypropylene composite modified material, and then adopting the polypropylene composite modified material to prepare a finished product of the medicine bottle by plasticating, injection molding, blow molding and demolding processes, wherein the plastic particles comprise: 80 parts of PP and 15 parts of LDPE. However, the performance of the oral liquid plastic bottle and the stability of the preparation are not clear.
At present, an oral liquid packaging container is still needed to meet the requirements of a terminal steam sterilization process in the production process, and is suitable for an oral liquid bottle with stable quality in the storage period of foods and medicines.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the composite food-grade oral liquid bottle and the preparation method thereof, wherein the oral liquid bottle cannot pollute food and medicines in the process of packaging and contacting the food and the medicines, cannot leak under the storage condition, and ensures the stable quality of the food and the medicines under the long-term storage condition. Specifically, the present invention includes the following.
The invention provides a composite food-grade oral liquid bottle, which comprises the following components in parts by weight:
70-90 parts of food-grade polypropylene resin, 5-15 parts of food-grade high-density polyethylene, 5-15 parts of food-grade polyphenylene sulfone and 0.5-1.0 part of modified color master batch. The inventor discovers through a large number of researches that too high or too low content of the components can cause the structure and the intermolecular distance of the plastic oral liquid bottle, influence the permeation of water molecules and further influence the performance of the plastic oral liquid bottle. Wherein the food-grade polypropylene resin is preferably 75-85 parts, more preferably 76-84 parts, still more preferably 78-82 parts, and most preferably 79-81 parts. The food-grade high-density polyethylene is preferably 6 to 13 parts, more preferably 7 to 12 parts, still more preferably 8 to 11 parts, and most preferably 9 to 11 parts. The food-grade polyphenylene sulfone is preferably 6 to 13 parts, more preferably 7 to 12 parts, still more preferably 8 to 11 parts, most preferably 9 to 11 parts. The modified color master batch is preferably 0.7 to 1.0 part, more preferably 0.8 to 1.0 part, still more preferably 0.9 to 1.0 part.
According to the composite food-grade oral liquid bottle, preferably, the modified color master batch is prepared by kneading and forming raw materials of polypropylene, polytetrafluoroethylene and titanium dioxide in a kneader, and granulating by an extruder. Also preferably, the polypropylene, polytetrafluoroethylene and titanium dioxide are 2-6 parts. Further preferably, the polypropylene, polytetrafluoroethylene and titanium dioxide are 4 parts of the composite food-grade oral liquid bottle according to the invention.
Preferably, the feedstock further comprises an auxiliary agent comprising a silane-terminated polyether based cross-linked polymer and a wax, wherein the silane-terminated polyether based cross-linked polymer is in the range of 0.01 to 0.03 parts. The wax includes, but is not limited to, a polyolefin wax selected from the group consisting of polyethylene waxes, polar polyethylene waxes, polypropylene waxes, polar polypropylene waxes, and mixtures thereof. The preferred wax is a polyethylene wax, and the polyethylene wax is 0.01 to 0.02 parts.
According to the composite food-grade oral liquid bottle, preferably, the temperature of a first region of a screw rod for granulating by an extruder is 230-250 ℃, the temperature of a second region is 210-230 ℃, the temperature of a third region is 190-210 ℃, the temperature of a fourth region is 180-190 ℃ and the temperature of a fifth region is 170-180 ℃. It is also preferred that the screw first zone temperature be 245 ℃, the second zone temperature be 225 ℃, the third zone temperature be 200 ℃, the fourth zone temperature be 185 ℃ and the fifth zone temperature be 175 ℃.
The composite food-grade oral liquid bottle according to the present invention preferably has a kneading molding temperature of 190-220 ℃ and a kneading molding time of 15-20min. It is also preferable that the kneading molding temperature is 200 to 210℃and the kneading molding time is 16 to 18 minutes.
In a second aspect of the present invention, there is provided a method of preparing a composite food grade oral liquid bottle, comprising at least the steps of:
(1) Feeding the compound components to a mixing cylinder through a feeding system to obtain a mixed material;
(2) The mixture is made into composite food-grade bottle blanks by a filling blow hollow forming machine.
According to the preparation method of the composite food-grade oral liquid bottle, in the step (2), preferably, the injection quantity (PS) of the injection blow hollow molding machine is controlled to be 240g, the pre-molding pressure is controlled to be 100-120MPa, the injection pressure is controlled to be 50-75MPa, the dwell time is controlled to be 0.5-15 seconds, the injection time is controlled to be 1.5-10 seconds, the blowing time is controlled to be 7.0-8.0 seconds, the exhausting time is controlled to be 0.5-1.0 seconds, and the blowing pressure is controlled to be 8.0-10.0MPa.
According to the preparation method of the composite food-grade oral liquid bottle, preferably, in the step (2), the molding temperature of the injection blow hollow molding machine is controlled to be: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C. It is also preferable that the molding temperature of the injection blow molding machine is controlled to be: the first region temperature is 240-245 ℃, the second region temperature is 215-225 ℃, the third region temperature is 200-205 ℃, the fourth region temperature is 185-190 ℃ and the fifth region temperature is 175-180 ℃.
According to the preparation method of the composite food-grade oral liquid bottle, preferably, the deformation rate and the leakage rate of the composite food-grade plastic oral liquid bottle prepared by the method are not higher than 3.5%, more preferably not higher than 2.0%, even more preferably not higher than 1.0%, even not higher than 0.5%, such as 0.3%, 0.2% and 0.1% at the temperature of 121 ℃ and the pressure of 0.21 MPa.
According to the preparation method of the composite food-grade oral liquid bottle, preferably, the water vapor permeability of the composite food-grade oral liquid bottle prepared by the method is 0.007-0.021% measured according to the 2015 drug pack standard YBB00082002-2015 oral liquid medical polypropylene bottle.
According to the preparation method of the composite food-grade oral liquid bottle, preferably, the composite food-grade oral liquid bottle prepared by the method has the strong alkali/acid weight loss rate of less than 0.073%, preferably less than 0.060%, still preferably less than 0.050% and even less than 0.040% measured according to GB/T11547-2008 determination of liquid chemical resistance of plastics.
In a third aspect of the present invention there is provided the use of a composite food grade oral liquid bottle according to the first aspect in packaging containers for oral dosage forms.
The invention prepares the high-strength oral liquid bottle with good acid resistance, alkali resistance and heat resistance through specific raw material proportion, is not only beneficial to the storage stability of the oral liquid dosage forms of medicines and health-care foods, but also solves the problem of broken glass slag quality risk caused by using the glass bottle, does not need cleaning and drying procedures under clean condition production conditions, greatly reduces the production cost, and has good application prospect in the field of liquid preparation packaging.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present invention, it is understood that the upper and lower limits of the ranges and each intermediate value therebetween are specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
In the present invention, the term food grade has the usual meaning in the art, refers to a material that is non-toxic and safe to the human body and can be used for the manufacture of plastic containers for food.
The raw materials of the invention including food-grade polypropylene resin, food-grade high density polyethylene, food-grade polyphenylene sulfone, polypropylene, polytetrafluoroethylene and titanium dioxide are commercially available or can be prepared by known methods. Adjuvants useful in the present invention include cross-linked polymers based on silane-terminated polyethers and waxes,wherein the crosslinked polymer based on the silane-terminated polyether can be prepared by known methods or obtained by commercial products, examples of which include, but are not limited toMS series products, etc.
In the present invention, the injection blow molding machine preferably has an injection mechanism, a mold clamping system, a mold release system to effect injection-blow one-step completion of the preparation of the packaging container, examples of such machines include, but are not limited to, injection blow molding machines such as model MSZ 60.
The composite food-grade plastic oral liquid bottle is suitable for packaging containers of liquid preparations, especially for packaging containers of children Qixing tea oral liquid, and experiments prove that the composite food-grade plastic oral liquid bottle has required compatibility and long-term stability.
It will be appreciated by those skilled in the art that other steps or operations may be included before and after steps (1) - (2) or between steps of the invention, as long as the objects of the invention are achieved, such as further optimizing and/or improving the process described herein.
Example 1
The embodiment exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 70 parts of food-grade polypropylene resin (PP), 15 parts of food-grade high-density polyethylene (HDPE), 15 parts of food-grade polyphenylene sulfone (PPSU) and 1.0 part of modified masterbatch (polypropylene, polytetrafluoroethylene and titanium dioxide). The preparation method of the modified color master batch specifically comprises the following steps:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the raw materials, mixing, wherein the auxiliary agent is a mixture of a cross-linked polymer of silane end capped polyether and polyethylene wax, the cross-linked polymer of the silane end capped polyether (namely, modified silane adhesive) is 0.01-0.03 part, and the polyethylene wax is 0.01-0.02 part;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: first zone temperature 240 ℃, second zone temperature 220 ℃, third zone temperature 200 ℃, fourth zone temperature 185 ℃ and fifth zone temperature 175 ℃.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, high-density polyethylene, polyphenylene sulfone and modified color master batch) materials into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of dwell time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure, inputting the prepared materials into a hopper, heating and melting the materials through a screw heating cylinder, injecting and blowing to form, preheating the plastics into a molten state through a cylinder of an injection and blowing machine, and controlling the temperature of the cylinder: front section: 240 ℃, middle section: 225 ℃, the later stage: and (3) automatically moving the tube blank to a bottle blowing die by a bottle blowing machine at 205 ℃ and 240 ℃ through a hot runner, closing the die, performing injection blow molding, opening the die, and taking off the product to obtain the bottle blank.
Example 2
The embodiment exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 80 parts of food-grade polypropylene resin (PP), 10 parts of food-grade high-density polyethylene (HDPE), 10 parts of food-grade polyphenylene sulfone (PPSU) and 1.0 part of modified masterbatch (polypropylene, polytetrafluoroethylene and titanium dioxide). The preparation method of the modified color master batch specifically comprises the following steps:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the component raw materials, and mixing;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, high-density polyethylene, polyphenylene sulfone and modified color master batch) materials into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of pressure maintaining time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure (the prepared materials are input into a hopper, heated and melted by a screw heating cylinder, injection-blow-molded, preheated by a cylinder of an injection-blow molding machine, so that plastics are in a molten state, the cylinder temperature is controlled to be 245 ℃ at the front section, 225 ℃ at the middle section and 250 ℃ at the rear section, the hot runner temperature is 250 ℃, a tube blank is formed, a bottle blowing machine automatically moves the tube blank to a bottle blowing mold, and after the injection-blow molding is carried out after the mold is closed, the mold is opened, and the product is removed, so that a bottle blank is obtained.
Example 3
The embodiment exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 90 parts of food-grade polypropylene resin (PP), 5 parts of food-grade high-density polyethylene (HDPE), 5 parts of food-grade polyphenylene sulfone (PPSU) and 1.0 part of modified masterbatch (polypropylene, polytetrafluoroethylene and titanium dioxide), wherein the preparation method of the modified masterbatch comprises the following specific steps of:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the component raw materials, and mixing;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, high-density polyethylene, polyphenylene sulfone and modified color master batch) materials into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of pressure maintaining time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure (the prepared materials are input into a hopper, heated and melted by a screw heating cylinder, injection-blow-molded, preheated by a cylinder of an injection-blow molding machine, so that plastics are in a molten state, the cylinder temperature is controlled to be 245 ℃ at the front section, 225 ℃ at the middle section and 250 ℃ at the rear section, the hot runner temperature is 250 ℃, a tube blank is formed, a bottle blowing machine automatically moves the tube blank to a bottle blowing mold, and after the injection-blow molding is carried out after the mold is closed, the mold is opened, and the product is removed, so that a bottle blank is obtained.
Comparative example 1
The comparative example exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 90 parts of food-grade polypropylene resin (PP), 10 parts of polyphenylene sulfone and 1.0 part of modified color master batch (polypropylene, polytetrafluoroethylene and titanium dioxide). The preparation method of the modified color master batch specifically comprises the following steps:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the component raw materials, and mixing;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, polyphenylene sulfone and modified color master particles) into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of pressure maintaining time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure (the prepared materials are input into a hopper, heated and melted by a screw heating cylinder, injection-blow-molded, preheated by a cylinder of an injection-blow molding machine, so that plastics are in a molten state, the cylinder temperature is controlled to be 245 ℃ at the front section, 225 ℃ at the middle section and 250 ℃ at the rear section, the hot runner temperature is 250 ℃, a tube blank is formed, a bottle blowing machine automatically moves the tube blank to a bottle blowing mold, and after the injection-blow molding is carried out after the mold is closed, the mold is opened, and the product is removed, so that a bottle blank is obtained.
Comparative example 2
The comparative example exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 90 parts of food-grade high-density polyethylene (HDPE), 10 parts of polyphenylene sulfone and 1.0 part of modified color master batch (polypropylene, polytetrafluoroethylene and titanium dioxide). The preparation method of the modified color master batch specifically comprises the following steps:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the component raw materials, and mixing;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, polyphenylene sulfone and modified color master particles) into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of pressure maintaining time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure (the prepared materials are input into a hopper, heated and melted by a screw heating cylinder, injection-blow-molded, preheated by a cylinder of an injection-blow molding machine, so that plastics are in a molten state, the cylinder temperature is controlled to be 245 ℃ at the front section, 225 ℃ at the middle section and 250 ℃ at the rear section, the hot runner temperature is 250 ℃, a tube blank is formed, a bottle blowing machine automatically moves the tube blank to a bottle blowing mold, and after the injection-blow molding is carried out after the mold is closed, the mold is opened, and the product is removed, so that a bottle blank is obtained.
Comparative example 3
The comparative example exemplarily shows a composite food-grade plastic oral liquid bottle, which comprises the following components in parts by weight: 50 parts of food-grade polypropylene resin (PP), 50 parts of food-grade high-density polyethylene (HDPE) and 1.0 part of modified masterbatch (polypropylene, polytetrafluoroethylene and titanium dioxide).
The preparation method of the modified color master batch specifically comprises the following steps:
A. weighing 4 parts of polypropylene, polytetrafluoroethylene, titanium dioxide and an auxiliary agent according to the weight parts of the component raw materials, and mixing;
B. putting the mixed raw materials into a kneader for kneading and molding;
C. extruding and granulating the formed raw materials by a double-screw extruder to obtain modified color master batch particles.
Key process control parameters; the temperature of the kneading molding is 190-220 ℃, and the kneading molding time is 15-20min. The screw temperature of the twin-screw extruder is: the first region temperature is 230-250deg.C, the second region temperature is 210-230deg.C, the third region temperature is 190-210 deg.C, the fourth region temperature is 180-190 deg.C, and the fifth region temperature is 170-180deg.C.
The preparation method of the composite food-grade plastic oral liquid bottle comprises the following specific steps:
A. the intelligent central feeding system conveys three (polypropylene, high-density polyethylene and modified color master batch) materials into a mixing cylinder according to the weight parts of the composition raw materials;
B. the mixed material is prepared from Vidama MSZ60, and the technological parameters are as follows: 240g of injection quantity (PS), 100-120MPa of pre-molding pressure, 50-75MPa of injection pressure, 0.5-15 seconds of pressure maintaining time, 1.5-10 seconds of injection time, 7.0-8.0 seconds of blowing time, 0.5-1.0 seconds of exhaust time and 8.0-10.0MPa of blowing pressure (the prepared materials are input into a hopper, heated and melted by a screw heating cylinder, injection-blow-molded, preheated by a cylinder of an injection-blow molding machine, so that plastics are in a molten state, the cylinder temperature is controlled to be 245 ℃ at the front section, 225 ℃ at the middle section and 250 ℃ at the rear section, the hot runner temperature is 250 ℃, a tube blank is formed, a bottle blowing machine automatically moves the tube blank to a bottle blowing mold, and after the injection-blow molding is carried out after the mold is closed, the mold is opened, and the product is removed, so that a bottle blank is obtained.
Test example 1
The medicine production quality management standard implementation guidelines clearly specify that: the oral liquid preparation must be subjected to terminal sterilization, and the production of oral liquid medicines and health products mostly adopts a steam sterilization method after filling and sealing, and the sterilization conditions are as follows: the oral liquid bottle must have good heat resistance and strength, and no deformation and leakage of appearance under the conditions of high temperature and high pressure sterilization with the sterilization temperature of 115 ℃ and the saturated steam pressure of 30min, the sterilization temperature of 0.17MPa or the sterilization temperature of 121 ℃, the retention time of 20min and the saturated steam pressure of 0.21 MPa.
Experimental protocol: 2000 pieces of each of example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 were taken, 50ml of the erythrosin aqueous solution was poured into 50.+ -. 0.5ml of the erythrosin aqueous solution, and the solution was sealed with a screw cap and placed in a stainless steel tray. A set of; taking example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, 1000 samples each at temperature: 115 ℃ pressure: sterilizing under 0.17MPa for 30 min. Another group; taking example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, 1000 samples each at temperature: pressure at 121 ℃): sterilizing under 0.21MPa for 20min, cooling to room temperature, and checking appearance deformation, sealing and leakage conditions of each test.
TABLE 1 high temperature high pressure (Heat resistance) test of composite food grade Plastic oral liquid bottles
Conclusion of the test: under the high-temperature sterilization process condition; the oral liquid bottle needs to bear high Wen Subian and external steam pressure and also bears the thermal expansion force of the solution in the bottle, and has good heat resistance under special process conditions. As can be seen from the deformation ratios and leakage ratios in table 1, comparative example 2> comparative example 3> comparative example 1> example 3> example 2, and example 2 has the best heat resistance strength performance, and is an ideal packaging container for oral liquid dosage forms.
Test example 2
The prevention of water vapor permeation and the evaluation of the packaging form of food and medical products are very important from the viewpoint of ensuring the quality of food and medical products, such as the main components are damaged and the content of liquid is reduced due to the water vapor permeation of the packaging materials, and the oral liquid dosage form must ensure excellent water vapor permeation resistance in shelf life. The physical index of the water vapor permeability of the medical polypropylene bottle is definitely regulated according to the drug package material standard YBB00082002-2015 of the new edition of 2015.
The specific experimental scheme is as follows:
water vapor permeability: taking a bottle body and a screw cap (15 sets are taken in example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3) respectively, tightly twisting and sealing, weighing (accurate to 1 mg), adding water with marked capacity, heat-sealing the bottle body and the bottle bottom, precisely weighing, standing for 14 days under the conditions that the relative humidity is 65% +/-5% and the temperature is 20+/-2 ℃, taking out the outside of the wiping bottle, and precisely weighing. The weight loss is less than or equal to 0.2 percent and more than 1 set of weight loss is more than 0.2 percent calculated according to the following formula.
The calculation formula is as follows: (W1-W2)/(W1-W0). Times.100%
Wherein: w0 is the weight (g) of the bottle body and the bottle cap;
w1- -weight of bottle and aqueous solution before test (g);
w2- -weight of bottle and aqueous solution after test (g)
Table 2-test of water vapor permeability of composite food grade plastic oral liquid bottle
| Test examples | Empty bottle water vapor permeability (%) | Carrier liquid water vapor permeability (%) |
| Example 1 | 0.013 | 0.018 |
| Example 2 | 0.007 | 0.011 |
| Example 3 | 0.015 | 0.021 |
| Comparative example 1 | 0.012 | 0.016 |
| Comparative example 2 | 0.197 | 0.221 |
| Comparative example 3 | 0.071 | 0.092 |
Conclusion of experiment:
in the embodiment 2, the composite component mainly made of polypropylene material has the advantages of lower water vapor permeability than other test examples, compact structure, reduced intermolecular distance, increased water molecule permeation difficulty, low water vapor permeability and lower solution loss in the bottle than other test examples.
Test example 3
The oral liquid has very complex medicine components, contains a large amount of organic acid and alkaloid, and has high requirement on acid and alkali corrosion resistance for directly contacted packaging containers.
Therefore, the test example adopts a test method of GB/T11547-2008 'determination of liquid resistance chemical reagent of plastics'.
The specific experimental scheme is as follows:
concentrated sulfuric acid (98%) and concentrated NaOH (40%) were chosen as the test medium. The test set temperature is 23 soil at 2 ℃, and the standard test period (one week). The bodies (example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3) were cut into 1X 1cm2 small square pieces, and each test example was not less than three. The amount of the test solution is calculated according to the total surface area of the test sample, at least 8ml of the test solution is needed per square centimeter, the test sample is completely soaked in the test solution, the test solution is stirred once every 24 hours, and at the end of the soaking period, the test solution is washed by using liquid which has no influence on the test sample and can be miscible with the test solution, and then the test solution is wiped by filter paper. And finally, calculating the weight loss rate of the sample,
the calculation formula is as follows: p (%) = (Mo-M)/MoX 100
P is the weight loss rate, mo is the initial mass of the test sample, and M is the mass of the test sample after being soaked in a medium.
Table 3-Corrosion resistance test of composite food grade plastic oral liquid bottle
| Test examples | Strong acid weight loss ratio (%) | Weight loss of strong base (%) |
| Example 1 | 0.073 | 0.062 |
| Example 2 | 0.061 | 0.046 |
| Example 3 | 0.065 | 0.056 |
| Comparative example 1 | 0.072 | 0.067 |
| Comparative example 2 | 0.076 | 0.069 |
| Comparative example 3 | 0.081 | 0.049 |
Conclusion of the test: the materials in the components of each test example are inert materials, the weight loss rate data change is not large after the components are soaked in acid-base conditions with high concentration for 7 days, and experimental data show that each test example has good corrosion resistance and is very suitable for packaging containers of medicine and food oral liquid dosage forms.
Test example 4
The quality of the medicine is naturally limited by the physical and chemical properties of the medicine itself, but the packaging material of the medicine plays a vital role in the stability of the medicine. The medicine packaging material, the container composition formula, the selected raw materials and auxiliary materials and the production process cannot influence the quality of the product, and the requirements of the general requirement guideline of medicine packaging materials, the stability test guideline of raw materials and medicine preparations and the polypropylene bottle standard (YBB 00082002-2015) of oral liquid medicine are met in the 2015 edition of Chinese pharmacopoeia.
To further verify the stability of the quality of the drug during storage period of the oral liquid bottle prepared in example 2, the following test was conducted.
Oral liquid experimental sample: the pediatric seven-star tea oral liquid of the 2020 edition of Chinese pharmacopoeia is taken as a sample.
Prescription: semen coicis 4170g, rice sprout 4170g, haw 2080g, lophatherum gracile 3130g, uncaria 1560g, cicada slough 520g and licorice 520g.
The preparation method comprises soaking the above seven materials in 70-80deg.C hot water twice for 0.5 hr each time, filtering, and mixing filtrates. Decocting the rest six materials with water twice (each for 2 hr), filtering, mixing filtrates, mixing with rice sprout medicinal liquid, and mixing. Concentrating to obtain fluid extract with relative density of 1.08-1.12 (55deg.C), adding ethanol to make alcohol content reach 50%, standing for 24 hr, filtering, and recovering ethanol from filtrate until no alcohol smell. Adding water to 5000ml, adjusting pH to 5.5-6.5 with 8% sodium hydroxide solution, standing, and filtering. Adding 1550g of single syrup and 20g of potassium sorbate into the filtrate, adding water to 10000ml, stirring uniformly, filtering, filling and sterilizing to obtain the final product.
Packaging container test sample: six batches of oral liquid bottles were prepared as in example 2: 2019101, 2019102, 2019103, 2019104, 2019105, 2019106;
four batches of pediatric seven-star tea oral liquid in the test example: 190601, 190602, 190603, 190604.
The specific experimental contents are as follows:
1. stability examination of the pediatric Qixing tea oral liquid on the bottle prepared in example 2.
1.1 taking three batches of oral liquid bottles prepared in example 2: 2019104, 2020105 and 2020106, the batch number of the infant Qixing tea oral liquid produced by filling is 190601, and the batch number of the package mark after filling is: 20190701, 20190702, 20190703.
Placing the test sample in a constant temperature and humidity box with the temperature of 45+/-2 ℃ and the relative humidity of 60+/-10%, standing for 14 days, taking out the content of the test sample, and performing appearance, tightness, vibration test and water vapor permeation test by referring to YBB00082002-2015, wherein the test results are shown in the table below.
1.2 taking three batches of oral liquid bottles prepared in example 2: 2019104, 2019105 and 2019106, the lot number of the packaged seven-star oral liquid for children is 1601111, and the lot number of the packaged package mark is: 20190704, 20190705, 20190706. Placing the test sample in a constant temperature and humidity box with the temperature of 40+/-2 ℃ and the relative humidity of 90+/-10%, standing for 14 days, taking out the test sample, pouring out the content, and performing appearance, tightness, vibration test and water vapor permeation test according to YBB00262002-2015, wherein the test results are shown in the table below.
2. Long-term stability test
Three batches of oral liquid bottles prepared in example 2 were taken: 2019101, 2019102, 2019103. The infant seven-star oral liquid batch numbers are 190601, 190602 and 190603 respectively. The labeling batch numbers of the filled medicine packages are 20190707, 20190708 and 20190709 respectively, namely three tested samples. Placing the three batches of test samples into a constant temperature and humidity box with the temperature of 25+/-2 ℃ and the relative humidity of 60+/-10%, placing for 12 months, taking out the test samples respectively at 0, 3, 6, 9 and 12 months, and detecting to determine the influence of the package on the effective period of the medicine. The experimental results are shown in the following table.
3. Acceleration test
Three batches of oral liquid bottles prepared in example 2 were taken: 2019101, 2019102, 2019103. The infant seven-star oral liquid batch numbers are 190601, 190602 and 190603 respectively. The labeling batch numbers of the filled medicine packages are 20190710, 20190711 and 20190712 respectively, namely three tested samples. Placing the three batches of test samples into a constant temperature and humidity box with the temperature of 40+/-2 ℃ and the relative humidity of 70+/-10%, standing for 6 months, taking out the test samples respectively at 0, 1, 2, 3 and 6 months, and detecting. The results of the experiments were examined in the following table to determine the effect of the package on the expiration date of the drug.
Experimental junction test conclusion:
after the oral liquid bottle package pediatric seven-star oral liquid prepared in the embodiment 2 is subjected to a compatibility test, the test result shows that the quality of the medicine packaging material and the quality of the medicine in the medicine packaging material are not obviously changed. The compatibility test result of the oral liquid bottle prepared in the example 2 and the pediatric seven-star oral liquid is proved to be satisfactory, and the oral liquid bottle prepared in the example 2 is proved to completely meet the requirement of a medicinal packaging container.
While the invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Various modifications or changes may be made to the exemplary embodiments of the present disclosure without departing from the scope or spirit of the invention. The scope of the claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions.
Claims (6)
1. A composite food-grade oral liquid bottle suitable for children's Qixing tea oral liquid is characterized by comprising the following compound components in parts by weight: 80 parts of food-grade polypropylene resin, 10 parts of food-grade high-density polyethylene, 5-15 parts of food-grade polyphenylene sulfone and 0.5-1.0 part of modified color master batch, wherein the modified color master batch is prepared by kneading and forming raw materials of polypropylene, polytetrafluoroethylene and titanium dioxide in a kneader and granulating by an extruder, the water vapor permeability of the composite food-grade oral liquid bottle measured according to 2015 pharmaceutical pack standard YBB00082002-2015 oral liquid medical polypropylene bottle is 0.007-0.021, and the strong alkali/acid weight loss ratio measured according to GB/T11547-2008 plastic liquid chemical resistance measurement is below 0.073%.
2. The composite food grade oral liquid bottle for pediatric Qixing tea oral liquid of claim 1 wherein the raw materials of the modified color master batch further comprise an auxiliary agent comprising a silane terminated polyether based cross-linked polymer and a wax.
3. The composite food grade oral liquid bottle for pediatric seven-star tea oral liquid of claim 1, wherein the screw of the extruder for granulating has a first zone temperature of 230-250 ℃, a second zone temperature of 210-230 ℃, a third zone temperature of 190-210 ℃, a fourth zone temperature of 180-190 ℃ and a fifth zone temperature of 170-180 ℃.
4. A method for preparing a composite food-grade oral liquid bottle suitable for pediatric Qixing tea oral liquid according to any one of claims 1-3, comprising the steps of:
(1) Feeding the compound components to a mixing cylinder through a feeding system to obtain a mixed material;
(2) And making the mixed material into a composite food-grade plastic bottle blank by an injection blow hollow molding machine.
5. The method for preparing a composite food-grade oral liquid bottle for pediatric Qixing tea oral liquid according to claim 4, wherein in the step (2), the injection amount of the injection blow molding machine is controlled to 240g, the pre-molding pressure is controlled to 100-120MPa, the injection pressure is controlled to 50-75MPa, the dwell time is controlled to 0.5-15 seconds, the injection time is controlled to 1.5-10 seconds, the air blowing time is controlled to 7.0-8.0 seconds, the air exhausting time is controlled to 0.5-1.0 seconds, and the air blowing pressure is controlled to 8.0-10.0MPa.
6. Use of a composite food grade oral liquid bottle according to any one of claims 1-3 in packaging containers for pediatric Qixing tea oral liquid.
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