CN108285581A - A kind of preparation method and applications of medical polypropylene composite material - Google Patents

A kind of preparation method and applications of medical polypropylene composite material Download PDF

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CN108285581A
CN108285581A CN201810173471.0A CN201810173471A CN108285581A CN 108285581 A CN108285581 A CN 108285581A CN 201810173471 A CN201810173471 A CN 201810173471A CN 108285581 A CN108285581 A CN 108285581A
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付主枝
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/10Transparent films; Clear coatings; Transparent materials
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2203/02Applications for biomedical use
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/06Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
    • CCHEMISTRY; METALLURGY
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/04Thermoplastic elastomer

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Abstract

The invention discloses a kind of preparation method and applications of medical polypropylene composite material, this method is used polypropylene, N cyclohexylthiophthalimides input reaction kettle high temperature stirs to get primary mix, again with diethyl phosphite, polycaprolactone is added to addition absolute ethyl alcohol in ultrasonic dispersers and is ultrasonically treated jointly, heating and thermal insulation, obtain sub-mixtures, then by Modification of Montmorillonite, it finally will be in sub-mixtures and modified montmorillonite used common input reaction kettle, ethylene propylene diene rubber and Tripolyglycerol monostearates are added, high-temperature stirring under conditions of inert gas shielding, then cools down and toughener and stabilizer is added, stir to get ultimate mixture, then it is sent to twin (double) screw extruder and carries out melt extruded, segmentation, packaging, sterilizing, finished composite material is obtained after cooling.The medical polypropylene composite material being prepared, transparency height, shock resistance, has a good application prospect on medical devices.

Description

A kind of preparation method and applications of medical polypropylene composite material
Technical field
The present invention relates to medical material tech fields, and in particular to a kind of preparation method of medical polypropylene composite material and It is applied.
Background technology
Polypropylene is a kind of thermoplastic resin, is one of current global five big general-purpose plastics, can be divided into isotactic polypropylene, nothing Three kinds of isotactic polypropylene and syndiotactic polypropylene.Polypropylene is a kind of semi-crystalline material, than the hardness and higher that polyethylene has bigger Fusing point.Since the polypropylene of homopolymerization type has certain brittleness, so polymerization is often commonly incorporated into 1~4% or higher amount Ethylene obtains the copolymer of polypropylene-polyethylene as comonomer.The polypropylene material of homopolymer type and copolymer type is all With excellent resistance to water soak, antiacid caustic corrosion and antilysis, syringe used in the country, shifting drop device etc. are medical at present Equipment is mainly made of polypropylene material.But polypropylene also have the shortcomings that it is apparent:Transparency be not very well, mobility not It is easy to produce static electricity etc. in high and low temperature poor toughness and process, it limits it and is more widely applied in field of medical materials.
Invention content
In order to solve the above technical problems, the present invention provides a kind of preparation method of medical polypropylene composite material and its answers With this method is used stirs to get primary by polypropylene, N- cyclohexylthiophthalimides input reaction kettle high temperature Mixture, then be added in ultrasonic dispersers and add at absolute ethyl alcohol progress ultrasound jointly with diethyl phosphite, polycaprolactone Reason, heating and thermal insulation, obtain sub-mixtures, then by Modification of Montmorillonite, finally by sub-mixtures with it is modified montmorillonite used common It puts into reaction kettle, ethylene propylene diene rubber and Tripolyglycerol monostearates, high temperature under conditions of inert gas shielding is added Stirring, then cools down and toughener and stabilizer is added, stir to get ultimate mixture, be then sent to twin (double) screw extruder Melt extruded, segmentation, packaging, sterilizing are carried out, finished composite material is obtained after cooling.The medical composite polypropylene material being prepared Material, transparency height, shock resistance, has a good application prospect on medical devices.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of medical polypropylene composite material, includes the following steps:
It (1), will be anti-by in 25-35 parts of 55-65 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles It answers kettle temperature degree to be increased to 100-110 DEG C, is stirred the mixture for equal by mechanical agitation under 150-200 revs/min of rate It is even, obtain primary mix;
(2) primary mix for obtaining step (1) and 16-20 parts of diethyl phosphite, 10-15 parts of polycaprolactone are common It is added in ultrasonic dispersers, adds the absolute ethyl alcohol of 2 times of quality of mixture, then adjusted with the HCl solution of 0.1mol/L PH to 5.0, is ultrasonically treated, and will be then ultrasonically treated mixture and is heated to 90-100 DEG C, and keep the temperature 90-120 minutes, and obtain secondary Grade mixture;
(3) 6-8 parts of montmorillonite is dried under the conditions of 80-90 DEG C, drying time is 6-8 hours, will then be dried Product is cooled to room temperature, then 12-18 parts of epoxidized soybean oil is added into desciccate after cooling, is placed in homogenizer, It is stirred 20-30 minutes with 800-1200 revs/min of speed, then stops stirring, a concentration of 4% permanganic acid is added dropwise thereto 1-2 parts of potassium solution continues stirring 20-30 minutes, obtains modified montmorillonite used after being added dropwise to complete;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 6-10 parts of ethylene propylene diene rubber, 4-6 parts of Tripolyglycerol monostearates are added, it will be anti-under conditions of inert gas shielding It answers temperature in the kettle to be warming up to 160-180 DEG C, pyroreaction 3-4 hours under agitation, is then down to reactor temperature 75-85 DEG C, 2-4 parts of toughener, 2-4 parts of stabilizer is added, stirs 30-40 minutes at such a temperature, obtains ultimate mixture;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, obtains just making compound Material;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
Further, being ultrasonically treated preferably with 40-60 points of the frequency ultrasound of 20-30kHz dispersion in the step (2) Clock.
Further, the toughener in the step (4) is selected from ethylene-propylene-diene terpolymer, ethylene-vinegar Any one in sour ethylene copolymer, polyolefin thermoplastic elastomer.
Further, it is different to be selected from 1,1- diisopropoxies trimethylamine, phosphorous acid-benzene two for the stabilizer in the step (4) Any one in monooctyl ester, calcium stearate.
Further, the draw ratio of twin (double) screw extruder is 40-50 in the step (5):1, each silicon carbide is:First Section is 160-180 DEG C, and second interval is 180-190 DEG C, and 3rd interval is 195-205 DEG C.
Further, the invention also discloses medical polypropylene composite materials made from the preparation method answers in upper With.
Compared with prior art, the present invention advantage is:
(1) preparation method of medical polypropylene composite material of the invention is used polypropylene, N- cyclohexyl thio neighbour's benzene Dicarboximide input reaction kettle high temperature stirs to get primary mix, then adds jointly with diethyl phosphite, polycaprolactone Enter into ultrasonic dispersers addition absolute ethyl alcohol be ultrasonically treated, heating and thermal insulation, sub-mixtures are obtained, then by montmorillonite It is modified, finally by sub-mixtures and modified montmorillonite used common input reaction kettle, ethylene propylene diene rubber and three polyglycereol are added Monostearate, high-temperature stirring under conditions of inert gas shielding then cool down and toughener and stabilizer are added, stir To ultimate mixture, then it is sent to twin (double) screw extruder and carries out melt extruded, segmentation, packaging, sterilizing, obtained into after cooling Product composite material.The medical polypropylene composite material being prepared, transparency height, shock resistance have good on medical devices Good application prospect.
(2) present invention employs N- cyclohexylthiophthalimides, diethyl phosphite, polycaprolactone, modifications The participation of montmorillonite these types raw material prepares medical polypropylene composite material, and effective property has been carried out to medical polypropylene composite material It can be promoted, although these materials are not first Application in medical polypropylene composite material, according to a certain ratio after amount combination, It is aided with corresponding processing mode, is brought in performance significantly to the medical polypropylene composite material being finally prepared It improves, this is never to report in previous research, for realizing that the technique effect of the present invention plays conclusive work With.
Specific implementation mode
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 25 parts of 55 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 100 DEG C, is stirred the mixture for uniform by mechanical agitation under 150 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added to jointly with 16 parts of diethyl phosphite, 10 parts of polycaprolactone In ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, disperseed 40 minutes with the frequency ultrasound of 20kHz, will then be ultrasonically treated mixture and be heated to 90 DEG C, keep the temperature 90 minutes, obtain To sub-mixtures;
(3) 6 parts of montmorillonite is dried under the conditions of 80 DEG C, drying time is 6 hours, then cools down desciccate To room temperature, then 12 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 800 revs/min Speed stir 20 minutes, then stop stirring, a concentration of 4% 1 part of liquor potassic permanganate is added dropwise thereto, after being added dropwise to complete Continue stirring 20 minutes, obtains modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 6 parts of ethylene propylene diene rubber, 4 parts of Tripolyglycerol monostearates are added, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 160 DEG C, under agitation pyroreaction 3 hours, and reactor temperature is then down to 75 DEG C, and second is added Alkene -2 parts of acrylic-butadiene terpolymer, 2 parts of 1,1- diisopropoxies trimethylamine are stirred 30 minutes, are obtained at such a temperature Ultimate mixture;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 40:1, each silicon carbide is:First interval is 160 DEG C, and second interval is 180 DEG C, and 3rd interval is 195 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Embodiment 2
(1) by 30 parts of 60 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 105 DEG C, is stirred the mixture for uniform by mechanical agitation under 175 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added to jointly with 18 parts of diethyl phosphite, 12 parts of polycaprolactone In ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and be heated to 95 DEG C, keep the temperature 105 minutes, obtain To sub-mixtures;
(3) 7 parts of montmorillonite is dried under the conditions of 85 DEG C, drying time is 7 hours, then cools down desciccate To room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000 revs/min The speed of clock stirs 25 minutes, then stops stirring, a concentration of 4% 1.5 parts of liquor potassic permanganate is added dropwise thereto, drips Continue stirring 25 minutes after, obtains modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 8 parts of ethylene propylene diene rubber, 5 parts of Tripolyglycerol monostearates are added, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 170 DEG C, under agitation pyroreaction 3.5 hours, and reactor temperature is then down to 80 DEG C, and second is added 3 parts of alkene-acetate ethylene copolymer, 3 parts of Phenyl Di-2-ethyl Hexyl Phosphite stir 35 minutes, obtain ultimate mixing at such a temperature Object;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 45:1, each silicon carbide is:First interval is 170 DEG C, and second interval is 185 DEG C, and 3rd interval is 200 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Embodiment 3
(1) by 35 parts of 65 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 110 DEG C, is stirred the mixture for uniform by mechanical agitation under 200 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added to jointly with 20 parts of diethyl phosphite, 15 parts of polycaprolactone In ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, disperseed 60 minutes with the frequency ultrasound of 30kHz, will then be ultrasonically treated mixture and be heated to 100 DEG C, keep the temperature 120 minutes, Obtain sub-mixtures;
(3) 8 parts of montmorillonite is dried under the conditions of 90 DEG C, drying time is 8 hours, then cools down desciccate To room temperature, then 18 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1200 revs/min The speed of clock stirs 30 minutes, then stops stirring, a concentration of 4% 2 parts of liquor potassic permanganate is added dropwise thereto, is added dropwise to complete After continue stirring 30 minutes, obtain modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 10 parts of ethylene propylene diene rubber, 6 parts of Tripolyglycerol monostearates are added, by reaction kettle under conditions of inert gas shielding Interior temperature is warming up to 180 DEG C, under agitation pyroreaction 4 hours, and reactor temperature is then down to 85 DEG C, is added poly- 4 parts of olefinic thermoplastic elastomer, 4 parts of calcium stearate stir 40 minutes, obtain ultimate mixture at such a temperature;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 50:1, each silicon carbide is:First interval is 180 DEG C, and second interval is 190 DEG C, and 3rd interval is 205 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Comparative example 1
(1) by 60 parts of input reaction kettles of polypropylene, temperature of reaction kettle is increased to 105 DEG C, in 175 revs/min of speed Primary reaction object is obtained to uniform by mechanical agitation under rate;
(2) the primary reaction object that step (1) obtains is added to jointly with 18 parts of diethyl phosphite, 12 parts of polycaprolactone In ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and be heated to 95 DEG C, keep the temperature 105 minutes, obtain To sub-mixtures;
(3) 7 parts of montmorillonite is dried under the conditions of 85 DEG C, drying time is 7 hours, then cools down desciccate To room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000 revs/min The speed of clock stirs 25 minutes, then stops stirring, a concentration of 4% 1.5 parts of liquor potassic permanganate is added dropwise thereto, drips Continue stirring 25 minutes after, obtains modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 8 parts of ethylene propylene diene rubber, 5 parts of Tripolyglycerol monostearates are added, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 170 DEG C, under agitation pyroreaction 3.5 hours, and reactor temperature is then down to 80 DEG C, and second is added 3 parts of alkene-acetate ethylene copolymer, 3 parts of Phenyl Di-2-ethyl Hexyl Phosphite stir 35 minutes, obtain ultimate mixing at such a temperature Object;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 45:1, each silicon carbide is:First interval is 170 DEG C, and second interval is 185 DEG C, and 3rd interval is 200 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Comparative example 2
(1) by 30 parts of 60 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 105 DEG C, is stirred the mixture for uniform by mechanical agitation under 175 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added in ultrasonic dispersers jointly with 12 parts of polycaprolactone, then added Enter the absolute ethyl alcohol of 2 times of quality of mixture, pH to 5.0 is then adjusted with the HCl solution of 0.1mol/L, it is super with the frequency of 25kHz Sound disperses 50 minutes, will then be ultrasonically treated mixture and is heated to 95 DEG C, keeps the temperature 105 minutes, obtain sub-mixtures;
(3) 7 parts of montmorillonite is dried under the conditions of 85 DEG C, drying time is 7 hours, then cools down desciccate To room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000 revs/min The speed of clock stirs 25 minutes, then stops stirring, a concentration of 4% 1.5 parts of liquor potassic permanganate is added dropwise thereto, drips Continue stirring 25 minutes after, obtains modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 8 parts of ethylene propylene diene rubber, 5 parts of Tripolyglycerol monostearates are added, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 170 DEG C, under agitation pyroreaction 3.5 hours, and reactor temperature is then down to 80 DEG C, and second is added 3 parts of alkene-acetate ethylene copolymer, 3 parts of Phenyl Di-2-ethyl Hexyl Phosphite stir 35 minutes, obtain ultimate mixing at such a temperature Object;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 45:1, each silicon carbide is:First interval is 170 DEG C, and second interval is 185 DEG C, and 3rd interval is 200 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Comparative example 3
(1) by 30 parts of 60 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 105 DEG C, is stirred the mixture for uniform by mechanical agitation under 175 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added in ultrasonic dispersers jointly with 18 parts of diethyl phosphite, The absolute ethyl alcohol of 2 times of quality of mixture is added, pH to 5.0 is then adjusted with the HCl solution of 0.1mol/L, with the frequency of 25kHz Rate ultrasonic disperse 50 minutes will then be ultrasonically treated mixture and be heated to 95 DEG C, keeps the temperature 105 minutes, obtain sub-mixtures;
(3) 7 parts of montmorillonite is dried under the conditions of 85 DEG C, drying time is 7 hours, then cools down desciccate To room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000 revs/min The speed of clock stirs 25 minutes, then stops stirring, a concentration of 4% 1.5 parts of liquor potassic permanganate is added dropwise thereto, drips Continue stirring 25 minutes after, obtains modified montmorillonite used;
(4) the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains In, 8 parts of ethylene propylene diene rubber, 5 parts of Tripolyglycerol monostearates are added, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 170 DEG C, under agitation pyroreaction 3.5 hours, and reactor temperature is then down to 80 DEG C, and second is added 3 parts of alkene-acetate ethylene copolymer, 3 parts of Phenyl Di-2-ethyl Hexyl Phosphite stir 35 minutes, obtain ultimate mixing at such a temperature Object;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 45:1, each silicon carbide is:First interval is 170 DEG C, and second interval is 185 DEG C, and 3rd interval is 200 DEG C, Obtain just composite material processed;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Comparative example 4
(1) by 30 parts of 60 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, kettle temperature will be reacted Degree is increased to 105 DEG C, is stirred the mixture for uniform by mechanical agitation under 175 revs/min of rate, obtains primary mixing Object;
(2) primary mix that step (1) obtains is added to jointly with 18 parts of diethyl phosphite, 12 parts of polycaprolactone In ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and be heated to 95 DEG C, keep the temperature 105 minutes, obtain To sub-mixtures;
(3) sub-mixtures and montmorillonite that step (2) obtains are put into jointly in 7 parts of kettles of reaction, EPDM is added 8 parts of rubber, 5 parts of Tripolyglycerol monostearates, 170 are warming up under conditions of inert gas shielding by reactor temperature DEG C, pyroreaction 3.5 hours, are then down to 80 DEG C by reactor temperature under agitation, and it is total that ethene-vinyl acetate is added 3 parts of polymers, 3 parts of Phenyl Di-2-ethyl Hexyl Phosphite stir 35 minutes, obtain ultimate mixture at such a temperature;
(4) the ultimate mixture for obtaining step (3) is sent into twin (double) screw extruder and carries out melt extruded, twin (double) screw extruder Draw ratio be 45:1, each silicon carbide is:First interval is 170 DEG C, and second interval is 185 DEG C, and 3rd interval is 200 DEG C, Obtain just composite material processed;
(5) the first composite material processed that step (4) obtains is split, then the material divided is packed, is gone out Bacterium obtains finished composite material after cooling.
The performance test results of medical polypropylene composite material obtained are as shown in table 1.
Medical polypropylene composite material made from embodiment 1-3 and comparative example 1-4 is subjected to transparency, cantilever beam respectively This two performance tests of impact strength.
Table 1
Transparency (%) Cantilever beam impact strength (20 DEG C)
Embodiment 1 92 124
Embodiment 2 92 126
Embodiment 3 91 125
Comparative example 1 88 118
Comparative example 2 87 113
Comparative example 3 89 120
Comparative example 4 92 105
The preparation method of the medical polypropylene composite material of the present invention is used polypropylene, N- cyclohexyl thio O-phthalics Acid imide input reaction kettle high temperature stirs to get primary mix, then is added to jointly with diethyl phosphite, polycaprolactone In ultrasonic dispersers add absolute ethyl alcohol be ultrasonically treated, heating and thermal insulation, obtain sub-mixtures, then change montmorillonite Property, finally by sub-mixtures and modified montmorillonite used common input reaction kettle, ethylene propylene diene rubber and three polyglycereol lists are added Stearate, high-temperature stirring under conditions of inert gas shielding then cool down and toughener and stabilizer are added, stir to get Ultimate mixture is then sent to twin (double) screw extruder and carries out melt extruded, segmentation, packaging, sterilizing, finished product is obtained after cooling Composite material.The medical polypropylene composite material being prepared, transparency height, shock resistance have good on medical devices Application prospect.Also, present invention employs N- cyclohexylthiophthalimides, diethyl phosphite, polycaprolactone, Modified montmorillonite used these types raw material participation prepares medical polypropylene composite material, has been carried out effectively to medical polypropylene composite material Performance boost, although these materials are not first Application in medical polypropylene composite material, amount group according to a certain ratio After conjunction, it is aided with corresponding processing mode, is brought in performance to the medical polypropylene composite material being finally prepared It increases substantially, this is never to report in previous research, for realizing that the technique effect of the present invention plays decision The effect of property.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks Domain is included within the scope of the present invention.

Claims (6)

1. a kind of preparation method of medical polypropylene composite material, which is characterized in that include the following steps:
(1) by 25-35 parts of 55-65 parts of polypropylene, N- cyclohexylthiophthalimides input reaction kettles, by reaction kettle Temperature is increased to 100-110 DEG C, is stirred the mixture for uniform, is obtained by mechanical agitation under 150-200 revs/min of rate To primary mix;
(2) primary mix for obtaining step (1) and 16-20 parts of diethyl phosphite, the common addition of 10-15 parts of polycaprolactone Into ultrasonic dispersers, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl solution of 0.1mol/L adjust pH to 5.0, it is ultrasonically treated, will then be ultrasonically treated mixture and be heated to 90-100 DEG C, keep the temperature 90-120 minutes, obtained secondary mixed Close object;
(3) 6-8 parts of montmorillonite is dried under the conditions of 80-90 DEG C, drying time is 6-8 hours, then by desciccate It is cooled to room temperature, then adds 12-18 parts of epoxidized soybean oil into desciccate after cooling, be placed in homogenizer, with 800-1200 revs/min of speed stirs 20-30 minutes, then stops stirring, a concentration of 4% potassium permanganate is added dropwise thereto 1-2 parts of solution continues stirring 20-30 minutes, obtains modified montmorillonite used after being added dropwise to complete;
(4) in the modified montmorillonite used common input reaction kettle for obtaining sub-mixtures and step (3) that step (2) obtains, add Enter 6-10 parts of ethylene propylene diene rubber, 4-6 parts of Tripolyglycerol monostearates, it will be in reaction kettle under conditions of inert gas shielding Temperature is warming up to 160-180 DEG C, and pyroreaction 3-4 hours under agitation, reactor temperature is then down to 75-85 DEG C, 2-4 parts of toughener, 2-4 parts of stabilizer is added, stirs 30-40 minutes at such a temperature, obtains ultimate mixture;
(5) the ultimate mixture for obtaining step (4) is sent into twin (double) screw extruder and carries out melt extruded, obtains just composite wood processed Material;
(6) the first composite material processed that step (5) obtains is split, then the material divided is packed, is sterilized, it is cold But finished composite material is obtained afterwards.
2. the preparation method of medical polypropylene composite material according to claim 1, which is characterized in that the step (2) In be ultrasonically treated preferably with the frequency ultrasound of 20-30kHz disperse 40-60 minutes.
3. the preparation method of medical polypropylene composite material according to claim 1, which is characterized in that the step (4) In toughener be selected from ethylene-propylene-diene terpolymer, ethylene-vinyl acetate copolymer, polyolefine thermoplastic elastomer Any one in body.
4. the preparation method of medical polypropylene composite material according to claim 1, which is characterized in that the step (4) In any one in 1,1- diisopropoxies trimethylamine, Phenyl Di-2-ethyl Hexyl Phosphite, calcium stearate of stabilizer.
5. the preparation method of medical polypropylene composite material according to claim 1, which is characterized in that the step (5) The draw ratio of middle twin (double) screw extruder is 40-50:1, each silicon carbide is:First interval is 160-180 DEG C, and second interval is 180-190 DEG C, 3rd interval is 195-205 DEG C.
6. according to medical polypropylene composite material made from any one of the claim 1-5 preparation methods on medical devices Using.
CN201810173471.0A 2018-03-02 2018-03-02 A kind of preparation method and applications of medical polypropylene composite material Withdrawn CN108285581A (en)

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Application publication date: 20180717