CN108117687A - A kind of preparation method and applications for the medical composite material for adding fluorine silicone rubber - Google Patents
A kind of preparation method and applications for the medical composite material for adding fluorine silicone rubber Download PDFInfo
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- CN108117687A CN108117687A CN201810115599.1A CN201810115599A CN108117687A CN 108117687 A CN108117687 A CN 108117687A CN 201810115599 A CN201810115599 A CN 201810115599A CN 108117687 A CN108117687 A CN 108117687A
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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
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- C08L2203/02—Applications for biomedical use
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of preparation method and applications for the medical composite material for adding fluorine silicone rubber,This method is used polyethylene wax,N,N dimethyl cyclohexyl amines input reaction kettle high temperature stirs to get primary mix,Again with polyethylene terephthalate,Polycarbonate resin is added to addition absolute ethyl alcohol in ultrasonic dispersers and is ultrasonically treated jointly,Heating and thermal insulation,Obtain sub-mixtures,Then magnesium borate crystal whisker is modified,Finally sub-mixtures and boric acid modification magnesium whisker are put into reaction kettle jointly,Add in fluorine silicone rubber and cellulose acetate-butyrate,The high-temperature stirring under conditions of inert gas shielding,Then cool down and add in toughener and stabilizer,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 composite material for the addition fluorine silicone rubber being prepared, high mechanical strength, anti-steam performance are good, have a good application prospect on disposable infusion equipment.
Description
Technical field
The present invention relates to medical material tech fields, and in particular to a kind of system for the medical composite material for adding fluorine silicone rubber
Preparation Method and its application.
Background technology
It is well known that most disposable infusion equipment is usually all using igelite, polyvinyl chloride tool now
Have not that cracky, the transparency are high, the advantages that when normal use do not twist together, high temperature-resistant disinfected and good mechanical property.But polychlorostyrene second
There is also many defects simultaneously for alkene material：Minimal amount of vinyl chloride monomer is remained in polyvinyl chloride, which has been found
It is carcinogen；Polrvinyl chloride product has used dioctyl phthalate in processing, and as plasticizer, animal experiment shows
Dioctyl phthalate has the systems such as reproductive system, liver, lungs and angiocarpy different degrees of toxic action, gives people
Class health care belt carrys out risk；Polyvinyl chloride has suction-operated to some drugs, inaccurate using pharmaceutical quantities, affects the treatment；In addition,
Human body may be entered to people's in infusion process by making stabilizer added with a variety of compounds containing metal when polyvinyl chloride is processed
Health brings harm etc..Therefore, it is necessary to develop a kind of new medical material to substitute current polyvinyl chloride.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method for the medical composite material for adding fluorine silicone rubber
And its application, this method are used polyethylene wax, N, N- dimethyl cyclohexyl amines input reaction kettle high temperature stirs to get primary mixed
Object is closed, then is added to jointly in ultrasonic dispersers with polyethylene terephthalate, polycarbonate resin and adds absolute ethyl alcohol
Be ultrasonically treated, heating and thermal insulation, obtain sub-mixtures, be then modified magnesium borate crystal whisker, finally by sub-mixtures with
Boric acid modification magnesium whisker is put into reaction kettle jointly, fluorine silicone rubber and cellulose acetate-butyrate is added in, in inert gas shielding
Under the conditions of high-temperature stirring, then cool down and add in toughener and stabilizer, stir to get ultimate mixture, be then sent to double
Screw extruder carries out melt extruded, segmentation, packaging, sterilizing, and finished composite material is obtained after cooling.The addition fluorine being prepared
The medical composite material of silicon rubber, high mechanical strength, anti-steam performance are good, have good answer on disposable infusion equipment
Use prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method for the medical composite material for adding fluorine silicone rubber, comprises the following steps：
(1) by 55-65 parts of polyethylene wax, N, in 25-35 parts of input reaction kettles of N- dimethyl cyclohexyl amines, by temperature of reaction kettle
100-110 DEG C is increased to, is stirred the mixture under 150-200 revs/min of rate by mechanical agitation to uniform, is obtained just
Grade mixture；
(2) primary mix for obtaining step (1) and 16-20 parts of polyethylene terephthalate, polycarbonate resin
10-15 parts of fat is added in ultrasonic dispersers jointly, the absolute ethyl alcohol of 2 times of quality of mixture is added, then with 0.1mol/L
HCl solution adjust pH to 5.0, be ultrasonically treated, will then be ultrasonically treated mixture and be heated to 90-100 DEG C, keep the temperature 90-
120 minutes, obtain sub-mixtures；
(3) 6-8 parts of magnesium borate crystal whisker is dried under the conditions of 80-90 DEG C, drying time for 6-8 it is small when, then will
Desciccate is cooled to room temperature, then 12-18 parts of epoxidized soybean oil is added into desciccate after cooling, is placed in homogenizer
In, it is stirred 20-30 minutes with 800-1200 revs/min of speed, then stops stirring, the height that concentration is 4% is added dropwise thereto
1-2 parts of potassium manganate solution continues stirring 20-30 minutes, obtains boric acid modification magnesium whisker after being added dropwise to complete；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6-10 parts of fluorine silicone rubber, 4-6 parts of cellulose acetate-butyrate are added in, it will be in reaction kettle under conditions of inert gas shielding
Temperature is warming up to 160-180 DEG C, and when pyroreaction 3-4 is small under agitation, reactor temperature then is down to 75-85
DEG C, 2-4 parts of toughener, 2-4 parts of stabilizer are added in, 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, and it is compound to obtain just system
Material；
(6) the first composite material processed for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
Further, being ultrasonically treated in the step (2) preferably disperses 40-60 points with the frequency ultrasound of 20-30kHz
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 the medical composite materials that fluorine silicone rubber is added made from the preparation method to exist
Application on infusion apparatus.
Compared with prior art, the present invention its advantage is：
(1) preparation method of the medical composite material of addition fluorine silicone rubber of the invention is used polyethylene wax, N, N- bis-
Methyl cyclohexylamine input reaction kettle high temperature stirs to get primary mix, then with polyethylene terephthalate, poly- carbonic acid
Ester resin be added to jointly in ultrasonic dispersers add absolute ethyl alcohol be ultrasonically treated, heating and thermal insulation, obtain sub-mixtures,
Then magnesium borate crystal whisker is modified, finally puts into sub-mixtures and boric acid modification magnesium whisker in reaction kettle jointly, add in fluorine
Silicon rubber and cellulose acetate-butyrate, the high-temperature stirring under conditions of inert gas shielding, then cool down and add in toughener and
Stabilizer, stirs to get ultimate mixture, is then sent to twin (double) screw extruder and carries out melt extruded, segmentation, pack, go out
Bacterium obtains finished composite material after cooling.The medical composite material for the addition fluorine silicone rubber being prepared, high mechanical strength,
Anti- steam performance is good, has a good application prospect on disposable infusion equipment.
(2) present invention employs N, N- dimethyl cyclohexyl amines, polyethylene terephthalate, change polycarbonate resin
Property magnesium borate crystal whisker these types raw material participate in preparing the medical composite material of addition fluorine silicone rubber, to the medical of addition fluorine silicone rubber
Composite material has carried out effective performance boost, although these materials are not first Application in the medical compound of addition fluorine silicone rubber
In material, but it is aided with corresponding processing mode, to the addition fluorine silicone rubber being finally prepared after amount combination according to a certain ratio
Medical composite material bring increasing substantially in performance, this is never to report in previous research, right
Play the role of in the technique effect for realizing the present invention conclusive.
Specific embodiment
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 55 parts of polyethylene wax, N, in 25 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 100 DEG C, is stirred the mixture under 150 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) and 16 parts of polyethylene terephthalate, polycarbonate resin 10
Part is added in ultrasonic dispersers jointly, adds the absolute ethyl alcohol of 2 times of quality of mixture, then molten with the HCl of 0.1mol/L
Liquid adjusts pH to 5.0, is disperseed 40 minutes with the frequency ultrasound of 20kHz, will then be ultrasonically treated mixture and is heated to 90 DEG C, heat preservation
90 minutes, obtain sub-mixtures；
(3) 6 parts of magnesium borate crystal whisker is dried under the conditions of 80 DEG C, drying time for 6 it is small when, then by desciccate
Be cooled to room temperature, then into desciccate after cooling add 12 parts of epoxidized soybean oil, be placed in homogenizer, with 800 turns/
The speed of minute stirs 20 minutes, then stops stirring, and 1 part of the liquor potassic permanganate that dropwise addition concentration is 4% thereto drips
Continue stirring 20 minutes after, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6 parts of fluorine silicone rubber, 4 parts of cellulose acetate-butyrate are added in, by reactor temperature liter under conditions of inert gas shielding
Temperature is to 160 DEG C, and when pyroreaction 3 is small under agitation, reactor temperature then is down to 75 DEG C, add in ethylene-propylene-
2 parts of butadiene terpolymer, 2 parts of 1,1- diisopropoxies trimethylamine stir 30 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 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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Embodiment 2
(1) by 60 parts of polyethylene wax, N, in 30 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 105 DEG C, is stirred the mixture under 175 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) and 18 parts of polyethylene terephthalate, polycarbonate resin 12
Part is added in ultrasonic dispersers jointly, adds the absolute ethyl alcohol of 2 times of quality of mixture, then molten with the HCl of 0.1mol/L
Liquid adjusts pH to 5.0, is disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and is heated to 95 DEG C, heat preservation
105 minutes, obtain sub-mixtures；
(3) 7 parts of magnesium borate crystal whisker is dried under the conditions of 85 DEG C, drying time for 7 it is small when, then by desciccate
It is cooled to room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000
Rev/min speed stir 25 minutes, then stop stirring, thereto be added dropwise concentration be 4% 1.5 parts of liquor potassic permanganate,
Continue stirring 25 minutes after being added dropwise to complete, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6-10 parts of fluorine silicone rubber, 5 parts of cellulose acetate-butyrate are added in, it will be warm in reaction kettle under conditions of inert gas shielding
Degree is warming up to 170 DEG C, and when pyroreaction 3.5 is small under agitation, reactor temperature then is down to 80 DEG C, adds in second
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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Embodiment 3
(1) by 65 parts of polyethylene wax, N, in 35 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 110 DEG C, is stirred the mixture under 200 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) and 20 parts of polyethylene terephthalate, polycarbonate resin 15
Part is added in ultrasonic dispersers jointly, adds the absolute ethyl alcohol of 2 times of quality of mixture, then molten with the HCl of 0.1mol/L
Liquid adjusts pH to 5.0, is disperseed 60 minutes with the frequency ultrasound of 30kHz, will then be ultrasonically treated mixture and is heated to 100 DEG C, protects
Temperature 120 minutes, obtains sub-mixtures；
(3) 8 parts of magnesium borate crystal whisker is dried under the conditions of 90 DEG C, drying time for 8 it is small when, then by desciccate
It is cooled to room temperature, then 18 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1200
Rev/min speed stir 30 minutes, then stop stirring, thereto be added dropwise concentration be 4% 2 parts of liquor potassic permanganate, drop
Continue stirring 30 minutes after adding into, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 10 parts of fluorine silicone rubber, 6 parts of cellulose acetate-butyrate are added in, by reactor temperature under conditions of inert gas shielding
180 DEG C are warming up to, when pyroreaction 4 is small under agitation, reactor temperature is then down to 85 DEG C, adds in polyolefin heat
4 parts of thermoplastic elastic, 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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Comparative example 1
(1) by 60 parts of input reaction kettles of polyethylene wax, temperature of reaction kettle is increased to 105 DEG C, at 175 revs/min
Mechanical agitation obtains primary reaction object to uniform under rate；
(2) the primary reaction object for obtaining step (1) and 18 parts of polyethylene terephthalate, polycarbonate resin 12
Part is added in ultrasonic dispersers jointly, adds the absolute ethyl alcohol of 2 times of quality of mixture, then molten with the HCl of 0.1mol/L
Liquid adjusts pH to 5.0, is disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and is heated to 95 DEG C, heat preservation
105 minutes, obtain sub-mixtures；
(3) 7 parts of magnesium borate crystal whisker is dried under the conditions of 85 DEG C, drying time for 7 it is small when, then by desciccate
It is cooled to room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000
Rev/min speed stir 25 minutes, then stop stirring, thereto be added dropwise concentration be 4% 1.5 parts of liquor potassic permanganate,
Continue stirring 25 minutes after being added dropwise to complete, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6-10 parts of fluorine silicone rubber, 5 parts of cellulose acetate-butyrate are added in, it will be warm in reaction kettle under conditions of inert gas shielding
Degree is warming up to 170 DEG C, and when pyroreaction 3.5 is small under agitation, reactor temperature then is down to 80 DEG C, adds in second
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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Comparative example 2
(1) by 60 parts of polyethylene wax, N, in 30 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 105 DEG C, is stirred the mixture under 175 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) is added in ultrasonic dispersers jointly with 12 parts of polycarbonate resin,
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 magnesium borate crystal whisker is dried under the conditions of 85 DEG C, drying time for 7 it is small when, then by desciccate
It is cooled to room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000
Rev/min speed stir 25 minutes, then stop stirring, thereto be added dropwise concentration be 4% 1.5 parts of liquor potassic permanganate,
Continue stirring 25 minutes after being added dropwise to complete, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6-10 parts of fluorine silicone rubber, 5 parts of cellulose acetate-butyrate are added in, it will be warm in reaction kettle under conditions of inert gas shielding
Degree is warming up to 170 DEG C, and when pyroreaction 3.5 is small under agitation, reactor temperature then is down to 80 DEG C, adds in second
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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Comparative example 3
(1) by 60 parts of polyethylene wax, N, in 30 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 105 DEG C, is stirred the mixture under 175 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) is added to ultrasound jointly with 18 parts of polyethylene terephthalate
In disperser, 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 ultrasound of 25kHz disperses 50 minutes, will then be ultrasonically treated mixture and is heated to 95 DEG C, keeps the temperature 105 minutes, obtain secondary
Mixture；
(3) 7 parts of magnesium borate crystal whisker is dried under the conditions of 85 DEG C, drying time for 7 it is small when, then by desciccate
It is cooled to room temperature, then 15 parts of epoxidized soybean oil is added into desciccate after cooling, be placed in homogenizer, with 1000
Rev/min speed stir 25 minutes, then stop stirring, thereto be added dropwise concentration be 4% 1.5 parts of liquor potassic permanganate,
Continue stirring 25 minutes after being added dropwise to complete, obtain boric acid modification magnesium whisker；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction jointly
In kettle, 6-10 parts of fluorine silicone rubber, 5 parts of cellulose acetate-butyrate are added in, it will be warm in reaction kettle under conditions of inert gas shielding
Degree is warming up to 170 DEG C, and when pyroreaction 3.5 is small under agitation, reactor temperature then is down to 80 DEG C, adds in second
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 for obtaining step (5) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling.
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
Comparative example 4
(1) by 60 parts of polyethylene wax, N, in 30 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is increased to
It 105 DEG C, is stirred the mixture under 175 revs/min of rate by mechanical agitation to uniform, obtains primary mix；
(2) primary mix for obtaining step (1) and 18 parts of polyethylene terephthalate, polycarbonate resin 12
Part is added in ultrasonic dispersers jointly, adds the absolute ethyl alcohol of 2 times of quality of mixture, then molten with the HCl of 0.1mol/L
Liquid adjusts pH to 5.0, is disperseed 50 minutes with the frequency ultrasound of 25kHz, will then be ultrasonically treated mixture and is heated to 95 DEG C, heat preservation
105 minutes, obtain sub-mixtures；
(3) in the common input reaction kettle of 7 parts of sub-mixtures and magnesium borate crystal whisker obtained step (2), fluorine silicon is added in
6-10 parts of rubber, 5 parts of cellulose acetate-butyrate, 170 DEG C are warming up under conditions of inert gas shielding by reactor temperature,
When pyroreaction 3.5 is small under agitation, reactor temperature is then down to 80 DEG C, adds in ethene-vinyl acetate copolymerization
3 parts of object, 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 for obtaining step (4) is split, and then packs the material split, goes out
Bacterium obtains finished composite material after cooling
The performance test results of the medical composite material of addition fluorine silicone rubber obtained are as shown in table 1.
The medical composite material of the addition fluorine silicone rubber obtained of embodiment 1-3 and comparative example 1-4 is stretched respectively
Intensity (GB/T 1040), shore hardness (GB/T 2411) and anti-vapor permeability (GB/T 10010) this several performance tests.
Table 1
The preparation method of the medical composite material of the addition fluorine silicone rubber of the present invention is used polyethylene wax, N, N- dimethyl
Cyclohexylamine input reaction kettle high temperature stirs to get primary mix, then with polyethylene terephthalate, polycarbonate resin
Fat be added to jointly in ultrasonic dispersers add absolute ethyl alcohol be ultrasonically treated, heating and thermal insulation, obtain sub-mixtures, then
Magnesium borate crystal whisker is modified, finally puts into sub-mixtures and boric acid modification magnesium whisker in reaction kettle jointly, adds in fluorine silicon rubber
Glue and cellulose acetate-butyrate, the high-temperature stirring under conditions of inert gas shielding then cool down and add in toughener and stabilization
Agent, stirs to get ultimate mixture, is then sent to twin (double) screw extruder and carries out melt extruded, segmentation, packaging, sterilizing, cold
But finished composite material is obtained afterwards.The medical composite material for the addition fluorine silicone rubber being prepared, high mechanical strength, anti-steam
Performance is good, has a good application prospect on disposable infusion equipment.Also, present invention employs N, N- dimethyleyelohexanes
Amine, polyethylene terephthalate, polycarbonate resin, boric acid modification magnesium whisker these types raw material participate in preparing addition fluorine silicon
The medical composite material of rubber has carried out effective performance boost to the medical composite material for adding fluorine silicone rubber, although these
Material is not first Application in the medical composite material of addition fluorine silicone rubber, but is aided with phase after amount combination according to a certain ratio
The processing mode answered is brought in performance significantly to the medical composite material for the addition fluorine silicone rubber being finally prepared
Degree improves, this is never to report in previous research, is played for the technique effect for realizing the present invention conclusive
Effect.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. a kind of preparation method for the medical composite material for adding fluorine silicone rubber, which is characterized in that comprise the following steps：
(1) by 55-65 parts of polyethylene wax, N, in 25-35 parts of input reaction kettles of N- dimethyl cyclohexyl amines, temperature of reaction kettle is raised
It to 100-110 DEG C, is stirred the mixture for uniform, obtained primary mixed by mechanical agitation under 150-200 revs/min of rate
Close object；
(2) primary mix for obtaining step (1) and 16-20 parts of polyethylene terephthalate, polycarbonate resin 10-
15 parts are added in ultrasonic dispersers jointly, add the absolute ethyl alcohol of 2 times of quality of mixture, then with the HCl of 0.1mol/L
Solution adjusts pH to 5.0, is ultrasonically treated, and will then be ultrasonically treated mixture and is heated to 90-100 DEG C, 90-120 points of heat preservation
Clock obtains sub-mixtures；
(3) 6-8 parts of magnesium borate crystal whisker is dried under the conditions of 80-90 DEG C, drying time for 6-8 it is small when, then by drying
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, the permanganic acid that concentration is 4% is added dropwise thereto
1-2 parts of potassium solution continues stirring 20-30 minutes, obtains boric acid modification magnesium whisker after being added dropwise to complete；
(4) the boric acid modification magnesium whisker that the sub-mixtures and step (3) obtained step (2) obtain puts into reaction kettle jointly
In, 6-10 parts of fluorine silicone rubber, 4-6 parts of cellulose acetate-butyrate are added in, it will be warm in reaction kettle under conditions of inert gas shielding
Degree is warming up to 160-180 DEG C, and when pyroreaction 3-4 is small under agitation, reactor temperature then is down to 75-85 DEG C,
2-4 parts of toughener, 2-4 parts of stabilizer are added in, 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 for obtaining step (5) is split, and then packs the material split, sterilizes, cold
But finished composite material is obtained afterwards.
2. the preparation method of the medical composite material of addition fluorine silicone rubber according to claim 1, which is characterized in that described
Supersound process in step (2) is preferably disperseed 40-60 minutes with the frequency ultrasound of 20-30kHz.
3. the preparation method of the medical composite material of addition fluorine silicone rubber according to claim 1, which is characterized in that described
Toughener in step (4) is selected from ethylene-propylene-diene terpolymer, ethylene-vinyl acetate copolymer, polyolefin heat
Any one in thermoplastic elastic.
4. the preparation method of the medical composite material of addition fluorine silicone rubber according to claim 1, which is characterized in that described
Stabilizer in step (4) is arbitrary in 1,1- diisopropoxies trimethylamine, Phenyl Di-2-ethyl Hexyl Phosphite, calcium stearate
It is a kind of.
5. the preparation method of the medical composite material of addition fluorine silicone rubber according to claim 1, which is characterized in that described
The draw ratio of twin (double) screw extruder is 40-50 in step (5):1, each silicon carbide is：First interval be 160-180 DEG C, second
Section is 180-190 DEG C, and 3rd interval is 195-205 DEG C.
6. the medical composite material of fluorine silicone rubber is added according to made from any one of the claim 1-5 preparation methods once
Application on property infusion apparatus.
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