CN109294242B - Material for infant aerosol inhaler and preparation method thereof - Google Patents

Material for infant aerosol inhaler and preparation method thereof Download PDF

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CN109294242B
CN109294242B CN201810967035.0A CN201810967035A CN109294242B CN 109294242 B CN109294242 B CN 109294242B CN 201810967035 A CN201810967035 A CN 201810967035A CN 109294242 B CN109294242 B CN 109294242B
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infant
aerosol inhaler
silicone oil
condensation polymer
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CN109294242A (en
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万迎春
邓生卫
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RUNSHENG PHARMACY Co.,Ltd.
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Runsheng Pharmacy Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/10Block- or graft-copolymers containing polysiloxane sequences
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/22Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/24Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/22Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/26Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42Block-or graft-polymers containing polysiloxane sequences
    • C08G77/44Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/02Applications for biomedical use
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/04Thermoplastic elastomer

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

The invention discloses a preparation method of a material for an infant aerosol inhaler, which comprises the following steps: preparing a fluorine-silicon condensation polymer; (II) single-end epoxy silicone oil modified fluorine-silicon condensation polymer; (III) mixing; and (IV) forming. The invention also discloses the material for the infant aerosol inhaler prepared by the preparation method. The material for the infant aerosol inhalation device disclosed by the invention has high texture simulation degree with mother breasts, excellent tear resistance, stretch resistance, ageing resistance, high temperature resistance and rebound resilience, can improve the compliance of infant aerosol inhalation treatment, can be matched with medical treatment to the maximum extent, has moderate softness and no toxicity, and cannot damage oral mucosa due to frequent movement of infants.

Description

Material for infant aerosol inhaler and preparation method thereof
Technical Field
The invention relates to the technical field of medical appliances, in particular to a material for an infant aerosol inhaler and a preparation method thereof.
Background
The aerosol inhalation therapy has become the first choice for treating various upper and lower respiratory system diseases in the global scope, such as common cold, fever, cough, asthma, sore throat, pharyngitis, rhinitis, bronchitis, pneumoconiosis and other diseases in trachea, bronchus, alveolus and thoracic cavity, and is also the conventional treatment method for infantile respiratory diseases. When the medical atomizer is applied to infants, the sick infants feel feared and cry and do not match with the sounds and the sprays generated in the atomization process due to the particularity of the psychology and the physiology of the infants, and the mouth of the existing medical atomizer is poor in performance of the prepared material, larger in hardness, difficult to disinfect, easy to age and has the defects of rubber smell, so that the treatment cannot be continued, the medicines are wasted, and the curative effect is influenced. Only invasive treatment modes such as intravenous administration and the like can be added, so that the pain and medical risk of the children are increased.
The breast milk simulated mouth made of the proper materials can eliminate the fear of infants, so that the infants can be matched with medical treatment to the maximum extent, and the compliance of the aerosol inhalation treatment of the infants is improved. In the prior art, the material of the mouth mainly comprises three types of rubber, latex and silica gel, the rubber mouth has rubber smell, the formula of the rubber compound is difficult to adjust and easy to yellow, and a vulcanizing agent contains sulfur and is harmful to human bodies; the latex mouth has good softness and elasticity, but generally has a slight rubber taste, the color is gradually deepened in the using process, the high-temperature resistance is poor, and the latex mouth is easy to age, so the using period is short; the buccal mouth of silica gel can resist temperature change, can be boiled, has smooth surface, is transparent, tasteless and good aging resistance, but the silica gel has poor elasticity, harder surface and poor tear resistance.
Therefore, the material for the mouth nozzle of the breast milk simulation infant inhalator, which has high simulation degree with the breast of a mother, excellent tear resistance, stretch resistance, aging resistance, high temperature resistance and rebound resilience and moderate hardness, is developed to meet the market demand and has wide market value.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a material for a buccal mouth of an infant inhalator and a preparation method thereof, and the preparation method has simple process and easy operation; through the molecular structure design, the material has high texture simulation degree with the mother breast, excellent tear resistance, stretch resistance, ageing resistance, high temperature resistance and rebound resilience, can improve the compliance of the aerosol inhalation treatment of the infants, enables the infants to be matched with the medical treatment to the maximum extent, has moderate softness and no toxicity, and does not damage oral mucosa due to frequent movement of the infants.
In order to achieve the aim, the technical scheme adopted by the invention is that the preparation method of the material for the infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving bis (chloromethyl) tetramethyldisilazane and bis (3-amino-4-fluorophenyl) ketone in a high-boiling-point solvent, adding an alkaline catalyst, stirring at 60-80 ℃ for reaction for 15-20 hours, adding 1-aminobenzotriazole, continuing stirring for 1-2 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 3-5 times, and finally drying in a vacuum drying oven at 90-100 ℃ for 12-18 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving the fluorosilicone condensation polymer prepared in the step I in dimethyl sulfoxide to form a solution, adding single-ended epoxy silicone oil and a catalyst, stirring and reacting for 10-15 hours at 80-90 ℃, then performing rotary evaporation to remove the solvent, washing for 3-5 times by using isopropanol, and then placing in a vacuum drying oven for drying for 10-15 hours at 50-60 ℃ to obtain the single-ended epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting the single-end epoxy silicone oil modified fluorine-silicon polycondensate prepared in the step II and the thermoplastic polyurethane elastomer into an open mill for mixing, adding an organic amine catalyst, performing triangular wrapping and rolling for 3-5 times respectively, and discharging and standing for later use;
IV, forming: and (3) placing the film prepared in the step (III) in a mould, placing the mould in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler.
Preferably, the mass ratio of the bis (chloromethyl) tetramethyldisilazane, the bis (3-amino-4-fluorophenyl) ketone, the high boiling point solvent, the alkaline catalyst and the 1-aminobenzotriazole in the step I is 1:1 (6-10): 0.3-0.5: 0.1.
Preferably, the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, the alkaline catalyst is selected from one or more of potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide.
Preferably, the mass ratio of the fluorine-silicon condensation polymer, the dimethyl sulfoxide, the single-end epoxy silicone oil and the catalyst in the step II is 1 (3-5): 0.3-0.5): 0.1.
Preferably, the catalyst is selected from at least one of triethylamine and tetrabutylammonium bromide.
Preferably, the mass ratio of the single-ended epoxy silicone oil modified fluorosilicone polycondensate, the thermoplastic polyurethane elastomer and the organic amine catalyst in the step III is 1 (0.4-0.7): 0.05.
Further, the organic amine catalyst is preferably triethylamine.
Further, in the step IV, the vacuum degree is 5 multiplied by 10-2-5×10-3Pa;The heating rate of the temperature rise is 20-40 ℃/min, and the temperature rise is up to 1500-; the pressurizing pressure is 2 x 107-4×107Pa; the heat preservation time of the heat preservation is 15-20 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1) the material for the mouth of the infant atomizing inhaler provided by the invention has the advantages of simple preparation method and process, easiness in operation, easiness in obtaining of used raw materials, moderate softness and no toxicity, and does not damage oral mucosa due to frequent movement of infants.
2) The material for the mouth of the infant nebulizer has the advantages that through the molecular structure design, the material and the mother breast have high texture simulation degree, and the material is excellent in tear resistance, stretch resistance, ageing resistance, high temperature resistance and rebound resilience, so that the compliance of infant nebulization inhalation treatment can be improved, and the infant nebulization inhaler can be matched with medical treatment to the maximum extent.
3) The material for the mouth of the infant atomizing inhaler provided by the invention contains the fluorine-silicon polycondensate, so that the comprehensive performance is more excellent, and the ultraviolet aging resistance of the material is improved by sealing the end of 1-aminobenzotriazole and introducing an aminobenzotriazole structure; the blend is obtained by blending the fluorine-silicon condensation polymer and the polyurethane thermoplastic elastomer, so that the material has the advantages of both the fluorine-silicon condensation polymer and the polyurethane thermoplastic elastomer, has excellent rebound resilience, high temperature resistance and tear resistance, and can be crosslinked during the forming process to form a three-dimensional network structure, thereby further improving the stability, high temperature resistance and tear resistance of the material; the fluorosilicone polycondensate is modified by the single-end epoxy silicone oil, and the long flexible chain segment is introduced, so that the resilience of the material is improved, and a certain stretching space is formed between molecular chains, so that the resilience is improved, the moderate softness of the material is ensured, the texture of the material is similar to that of a mother breast, and the treatment compliance of infants is improved.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
The raw material used in the following examples of the present invention was obtained from Shanghai spring Xin import & export trade company, Inc.
Example 1
A preparation method of a material for an infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving 100g of bis (chloromethyl) tetramethyldisilazane and 100g of bis (3-amino-4-fluorophenyl) ketone in 600g of dimethyl sulfoxide, adding 30g of potassium carbonate, stirring at 60 ℃ for reaction for 15 hours, adding 10g of 1-aminobenzotriazole, continuing stirring for 1 hour, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 3 times, and finally drying in a vacuum drying oven at 90 ℃ for 12 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving 100g of the fluorosilicone condensation polymer prepared in the step I in 300g of dimethyl sulfoxide to form a solution, adding 30g of single-ended epoxy silicone oil and 10g of triethylamine, stirring and reacting at 80 ℃ for 10 hours, then performing rotary evaporation to remove the solvent, washing with isopropanol for 3 times, and drying in a vacuum drying oven at 50 ℃ for 10 hours to obtain the single-ended epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting 100g of the single-end epoxy silicone oil modified fluorosilicone polycondensate prepared in the step II and 40g of the thermoplastic polyurethane elastomer into an open mill for mixing, adding 5g of triethylamine, performing triangular wrapping and rolling for 3 times respectively, and discharging and standing for later use;
IV, forming: will be prepared through step IIIPlacing the prepared film in a mold, placing in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler; the vacuum degree is 5 multiplied by 10-2Pa; the heating rate of the temperature rise is 20 ℃/min, and the temperature rise is up to 1500 ℃; the pressurizing pressure is 2 x 107Pa; the heat preservation time of the heat preservation is 15 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Example 2
A preparation method of a material for an infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving 100g of bis (chloromethyl) tetramethyldisilazane and 100g of bis (3-amino-4-fluorophenyl) ketone in 700g of N, N-dimethylformamide, adding 35g of sodium carbonate, stirring at 65 ℃ for reacting for 16 hours, adding 10g of 1-aminobenzotriazole, continuing stirring for 1.2 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 4 times, and finally drying in a vacuum drying oven at 92 ℃ for 13 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving 100g of the fluorosilicone condensation polymer prepared in the step I in 350g of dimethyl sulfoxide to form a solution, adding 35g of single-end epoxy silicone oil and 10g of tetrabutylammonium bromide, stirring and reacting at 83 ℃ for 12 hours, then performing rotary evaporation to remove the solvent, washing with isopropanol for 4 times, and then placing in a vacuum drying oven at 53 ℃ for drying for 11 hours to obtain the single-end epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting 100g of the single-end epoxy silicone oil modified fluorosilicone polycondensate prepared in the step II and 50g of the thermoplastic polyurethane elastomer into an open mill for mixing, adding 5g of triethylamine, performing triangular wrapping and rolling for 4 times respectively, and discharging and standing for later use;
IV, forming: placing the film prepared in the step III in a mold, placing the mold in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler; the vacuum degree is 3 multiplied by 10-2Pa; the heating rate of the temperature rise is 25 ℃/min, and the temperature rises to 1600 ℃; the pressurizing pressure is 2.5 multiplied by 107Pa; the heat preservation time of the heat preservation is 16 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Example 3
A preparation method of a material for an infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving 100g of bis (chloromethyl) tetramethyldisilazane and 100g of bis (3-amino-4-fluorophenyl) ketone in 800g of N-methylpyrrolidone, adding 40g of potassium hydroxide, stirring at 70 ℃ for reacting for 18 hours, adding 10g of 1-aminobenzotriazole, continuing stirring for 1.5 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 5 times, and finally drying in a vacuum drying oven at 95 ℃ for 15 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving 100g of the fluorosilicone condensation polymer prepared in the step I in 400g of dimethyl sulfoxide to form a solution, adding 40g of single-end epoxy silicone oil and 10g of triethylamine into the solution, stirring the solution at 85 ℃ for reaction for 13 hours, then performing rotary evaporation to remove the solvent, washing the solution with isopropanol for 5 times, and then drying the solution in a vacuum drying oven at 56 ℃ for 13.5 hours to obtain the single-end epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting 100g of the single-end epoxy silicone oil modified fluorosilicone polycondensate prepared in the step II and 60g of the thermoplastic polyurethane elastomer into an open mill for mixing, adding 5g of triethylamine, performing triangular wrapping and rolling for 5 times respectively, and discharging and standing for later use;
IV, forming: placing the film prepared in the step III in a mold, placing the mold in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler; the vacuum degree is 1 multiplied by 10-2Pa; the heating rate of the temperature rise is 30 ℃/min, and the temperature rise is 1800 ℃; the pressurizing pressure is 3 x 107Pa; the heat preservation time of the heat preservation is 18 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Example 4
A preparation method of a material for an infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving 100g of bis (chloromethyl) tetramethyldisilazane and 100g of bis (3-amino-4-fluorophenyl) ketone in 900g of a high-boiling-point solvent, adding 45g of an alkaline catalyst, stirring at 75 ℃ for reacting for 19 hours, adding 10g of 1-aminobenzotriazole, continuing stirring for 1.8 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 4 times, and finally drying at 98 ℃ in a vacuum drying oven for 17 hours to obtain a fluorine-silicon condensation polymer; the high-boiling-point solvent is a mixture formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 2:1: 3; the alkaline catalyst is a mixture formed by mixing potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide according to the mass ratio of 1:2:1: 3;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving 100g of the fluorosilicone condensation polymer prepared in the step I in 450g of dimethyl sulfoxide to form a solution, adding 45g of single-end epoxy silicone oil and 10g of a catalyst, stirring and reacting at 88 ℃ for 14 hours, then performing rotary evaporation to remove the solvent, washing with isopropanol for 4 times, and drying in a vacuum drying oven at 58 ℃ for 14 hours to obtain the single-end epoxy silicone oil modified fluorosilicone condensation polymer; the catalyst is a mixture formed by mixing triethylamine and tetrabutylammonium bromide according to the mass ratio of 3: 5;
III, mixing: putting 100g of the single-end epoxy silicone oil modified fluorosilicone polycondensate prepared in the step II and 65g of the thermoplastic polyurethane elastomer into an open mill for mixing, adding 5g of triethylamine, performing triangular wrapping and rolling for 5 times respectively, and discharging and standing for later use;
IV, forming: placing the film prepared in the step III in a mold, placing the mold in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler; the vacuum degree is 8 multiplied by 10-2Pa; the heating rate of the temperature rise is 35 ℃/min, and the temperature rise is up to 1900 ℃; the pressurizing pressure is 3.5 multiplied by 107Pa; the heat preservation time of the heat preservation is 19 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Example 5
A preparation method of a material for an infant aerosol inhaler comprises the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving 100g of bis (chloromethyl) tetramethyldisilazane and 100g of bis (3-amino-4-fluorophenyl) ketone in 1000g of dimethyl sulfoxide, adding 50g of potassium carbonate, stirring at 80 ℃ for reaction for 20 hours, adding 10g of 1-aminobenzotriazole, continuing stirring for 2 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 5 times, and finally drying in a vacuum drying oven at 100 ℃ for 18 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving 100g of the fluorosilicone condensation polymer prepared in the step I in 500g of dimethyl sulfoxide to form a solution, adding 50g of single-end epoxy silicone oil and 10g of tetrabutylammonium bromide, stirring and reacting at 90 ℃ for 15 hours, then performing rotary evaporation to remove the solvent, washing with isopropanol for 5 times, and then placing in a vacuum drying oven at 60 ℃ for drying for 15 hours to obtain the single-end epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting 100g of the single-end epoxy silicone oil modified fluorosilicone polycondensate prepared in the step II and 70g of the thermoplastic polyurethane elastomer into an open mill for mixing, adding 5g of triethylamine, performing triangular wrapping and rolling for 5 times respectively, and discharging and standing for later use;
IV, forming: placing the film prepared in the step III in a mold, placing the mold in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler; the vacuum degree is 5 multiplied by 10-3Pa; the heating rate of the temperature rise is 40 ℃/min, and the temperature rise is 2000 ℃; the pressurizing pressure is 4 x 107Pa; the heat preservation time of the heat preservation is 20 minutes.
A material for a buccal mouth of an infant aerosol inhaler is prepared by adopting the preparation method of the material for the infant aerosol inhaler.
The buccal mouth of the infant inhalator is prepared from the material for the buccal mouth of the infant inhalator.
An infant inhaler that adopts the mouth nozzle of the infant inhaler as the mouth nozzle.
Comparative example
The embodiment provides a breast milk true-proof polyethylene composite material, and the preparation method and the formula are the same as the embodiment 1 of the Chinese invention patent CN 10643289A.
The buccal mouths of the infant atomizing inhalers prepared in the embodiments 1-5 of the invention, the breast milk simulation polyethylene composite material in the comparative example 1 and the pure silica gel are respectively subjected to performance tests, and the test results and the method are shown in the table 1
TABLE 1
Figure BDA0001775228840000121
As can be seen from the above table, the mouth piece of the infant nebulizer disclosed in the embodiments of the present invention has more excellent mechanical properties and ultraviolet aging resistance, and has smaller hardness.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A preparation method of a material for an infant aerosol inhaler is characterized by comprising the following steps:
i preparation of fluorine-silicon condensation polymer: dissolving bis (chloromethyl) tetramethyldisilazane and bis (3-amino-4-fluorophenyl) ketone in a high-boiling-point solvent, adding an alkaline catalyst, stirring at 60-80 ℃ for reaction for 15-20 hours, adding 1-aminobenzotriazole, continuing stirring for 1-2 hours, cooling to room temperature, separating out in water, washing the separated polymer with ethanol for 3-5 times, and finally drying in a vacuum drying oven at 90-100 ℃ for 12-18 hours to obtain a fluorine-silicon condensation polymer;
II, single-end epoxy silicone oil modified fluorosilicone polycondensate: dissolving the fluorosilicone condensation polymer prepared in the step I in dimethyl sulfoxide to form a solution, adding single-ended epoxy silicone oil and a catalyst, stirring and reacting for 10-15 hours at 80-90 ℃, then performing rotary evaporation to remove the solvent, washing for 3-5 times by using isopropanol, and then placing in a vacuum drying oven for drying for 10-15 hours at 50-60 ℃ to obtain the single-ended epoxy silicone oil modified fluorosilicone condensation polymer;
III, mixing: putting the single-end epoxy silicone oil modified fluorine-silicon polycondensate prepared in the step II and the thermoplastic polyurethane elastomer into an open mill for mixing, adding an organic amine catalyst, performing triangular wrapping and rolling for 3-5 times respectively, and discharging and standing for later use;
IV, forming: and (3) placing the film prepared in the step (III) in a mould, placing the mould in a high-temperature furnace, vacuumizing, heating, pressurizing, preserving heat, and cooling to room temperature to obtain the material for the infant aerosol inhaler.
2. The method for preparing a material for an infant aerosol inhaler according to claim 1, wherein the mass ratio of bis (chloromethyl) tetramethyldisilazane, bis (3-amino-4-fluorophenyl) ketone, high boiling point solvent, basic catalyst and 1-aminobenzotriazole in step I is 1:1 (6-10): 0.3-0.5: 0.1.
3. The method for preparing a material for an infant aerosol inhaler according to claim 1, wherein the high boiling point solvent is one or more selected from dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
4. The method for preparing a material for an infant and pre-school children's aerosol inhaler according to claim 1, wherein the alkaline catalyst is one or more selected from potassium carbonate, sodium carbonate, potassium hydroxide and sodium hydroxide.
5. The method for preparing the material for the infant aerosol inhaler according to claim 1, wherein the mass ratio of the fluorine-silicon condensation polymer, the dimethyl sulfoxide, the single-end epoxy silicone oil and the catalyst in the step II is 1 (3-5) to 0.3-0.5) to 0.1; the catalyst is at least one of triethylamine and tetrabutylammonium bromide.
6. The method for preparing the material for the infant aerosol inhaler according to claim 1, wherein the mass ratio of the single-ended epoxy silicone oil modified fluorosilicone condensate, the thermoplastic polyurethane elastomer and the organic amine catalyst in step III is 1 (0.4-0.7) to 0.05; the organic amine catalyst is preferably triethylamine.
7. The method for preparing a material for an infant aerosol inhaler according to claim 1, wherein the vacuum is applied in step IV at a vacuum level of 5 x 10-2-5×10-3Pa; the heating rate of the temperature rise is 20-40 ℃/min, and the temperature rise is up to 1500-; the pressurizing pressure is 2 x 107-4×107Pa; the heat preservation time of the heat preservation is 15-20 minutes.
8. The material for the mouth of the infant aerosol inhaler, which is prepared by the preparation method of the material for the infant aerosol inhaler according to any one of claims 1 to 7.
9. An infant nebulizer mouthpiece made from the material for an infant nebulizer of claim 8.
10. An infant nebulizer that uses the infant nebulizer mouth of claim 9 as the mouth piece.
CN201810967035.0A 2018-08-23 2018-08-23 Material for infant aerosol inhaler and preparation method thereof Active CN109294242B (en)

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