CN109054743A - A kind of medical instrument absorbing material and preparation method thereof - Google Patents
A kind of medical instrument absorbing material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of medical instrument absorbing material, include the following steps: the preparation of the polyamide-based condensation polymer of (one) ferrocenyl, (2) preparation of cyano-thiophene class addition polymers, (3) the magnetic preparation for inhaling wave active constituent, (4) fullerene coated magnetic inhales wave active constituent, the preparation of (five) absorbing material.The invention also discloses the absorbing material being prepared according to the preparation method and using the absorbing material as the medical instrument of sheathing material.Disclosed by the invention preparation method is simple, and preparation cost is cheap；The medical instrument being prepared absorbing material has the advantages that absorbing property is good, absorption band is wide, good compatibility, light weight, thickness are thin, mechanical property and Good Heat-resistance.
Description
Technical field
The present invention relates to medical macromolecular materials technical fields, and in particular to a kind of medical instrument absorbing material and its system
Preparation Method.
Background technique
With the development of modern science and technology and electronics industry, more and more electromagenetic wave radiations are present in our week
Enclose, electromagenetic wave radiation increasingly increases the influence of the health of environment and people, such as airport, machine flight because Electromagnetic Interference without
Method is taken off and overdue, can often interfere the normal work of various electronic instrument for diagnosing and curing diseases devices in hospital, mobile phone, so as to cause test knot
Fruit the inaccuracy even generation of malpractice.To the health aspect of people, excessive electromagenetic wave radiation can cause nervous system, exempt from
Obstacle occurs for epidemic disease system, reproductive system and blood circulation system etc., in some instances it may even be possible to induce the serious disease including all kinds of cancers
Disease.It is chronically in electromagnetic wave environment, is damaged in human body by electromagnetic wave and has not enough time to the tissue of self-regeneration and the damage of organ
Wound can become dynamic disease change because of long-term accumulation, can threat to life when serious.
Absorbing material is a kind of material that can absorb the electromagnetic wave energy for projecting its surface, is precise electronic Medical treatment device
The security guard that tool works normally.Current common absorbing material can be divided into resistor-type, dielectric type and magnetic medium by wave principle is inhaled
Type.However these traditional generally existing suction waves of absorbing material are limited in scope, wave-absorbing effect needs the technical issues of being further increased,
And these materials will be applied in medical instrument, exist bad with basis material compatibility, dispersion is uneven, and stability of material is not
It is good, in the long-term use, it may appear that exosmose shortens service life, increases use cost.
Therefore, electromagnetic pollution is administered, a kind of absorbing material that can be kept out and weaken electromagenetic wave radiation is found, improves Medical treatment device
The measurement and use accuracy and safety of tool, it has also become urgent problem to be solved in the industry.
Summary of the invention
In order to overcome the defects of the prior art, the present invention is intended to provide a kind of medical instrument absorbing material and its preparation
Method, preparation method is simple for this, and preparation cost is cheap；The medical instrument suction wave being prepared by the preparation method
Material overcomes the existing wave of inhaling of traditional absorbing material and is limited in scope, and wave-absorbing effect needs the technical issues of being further increased, tool
Have absorbing property is good, absorption band is wide, good compatibility, light weight, thickness are thin, mechanical property and Good Heat-resistance it is excellent
Point.
The invention is realized by the following technical scheme: a kind of preparation method of medical instrument absorbing material, including as follows
Step:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: 1,1- diamino ferrocene, 2,5- thiophene dicarboxylic acid are added high
In boiling point solvent, 150-170 DEG C reaction 1-2 hours under normal pressure, then 1- ethyl-(3- dimethylaminopropyl) carbon is added thereto
Diimmonium salt hydrochlorate, 4-dimethylaminopyridine are warming up to 210-230 DEG C, and primary polycondensate reacts 5-7 hours, then by reaction solution
Be transferred in reaction kettle, vacuumize (500Pa), be heated to 240-250 DEG C, then polycondensation reaction 8-10 hours, after be precipitated in water, will
The polymer of precipitation is washed 3-5 times with acetone, then rotates removing acetone, obtains the polyamide-based condensation polymer of ferrocenyl；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile, 4- aminodiphenyl
Ethylene, initiator are dissolved in N-Methyl pyrrolidone, are stirred to react at nitrogen or 70-80 DEG C of atmosphere of inert gases 4-6 hours,
It is precipitated in water afterwards, and by the addition polymers of precipitation with ethanol washing 3-5 times, then is placed at 80-90 DEG C of vacuum oven dry 10-
15 hours, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: di-iron trioxide, yttrium oxide, lanthana, titanium oxide are mixed to get mixed
Material is closed, then is added to water and abrading-ball to mixture, carries out wet grinding 8-10 hours, is dried 2-4 at 110-120 DEG C
Hour, after be orientated in the magnetic field of 6000-9000A/m, after the pressure compression moulding of 18MPa-23Mpa, place into Muffle furnace
In be sintered, sintering temperature is 1000-1200 DEG C, with room temperature is furnace-cooled to after heat preservation 3-6 hour, obtain magnetic suction wave activity at
Point；
IV fullerene coated magnetic inhales wave active constituent: the magnetic wave active constituent of inhaling being prepared by step III is divided
Dissipate in ethyl alcohol, after chloromethyl triethoxysilane is added thereto, be stirred to react at 60-80 DEG C 4-6 hours, after again to it
It is middle that amino modified fullerene is added, continue to be stirred to react 6-8 hours, then filter, be washed 3-5 times with ethyl alcohol, then be placed in vacuum drying
It is 10-15 hours dry at 80-90 DEG C in case, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer of ferrocenyl being prepared by step I, by step
The II cyano-thiophene class addition polymers being prepared, the fullerene coated magnetic that is prepared by step IV inhale wave active constituent,
Metal organic frame is added in high-speed mixer, is made after high speed dispersion 20-40 minutes by extrusion shaping machine extrusion molding
Absorbing material.
Preferably, the ferrocene of 1,1- diamino described in step I, 2,5- thiophene dicarboxylic acid, high boiling solvent, 1- ethyl-
(3- dimethylaminopropyl) carbodiimide hydrochloride, 4-dimethylaminopyridine mass ratio be 1.25:1:(8-12): (0.4-
0.6):(0.2-0.3)。
Preferably, the high boiling solvent is in dimethyl sulfoxide, n,N-Dimethylformamide, N-Methyl pyrrolidone
It is one or more of.
Preferably, (2- thenylidene) methane -1,1'- dimethoxy nitrile described in step II, 4- amino-stilbene, initiation
Agent, N-Methyl pyrrolidone mass ratio be 1:1:(0.01-0.02): (8-12).
Preferably, the initiator is selected from least one of azodiisobutyronitrile, azobisisoheptonitrile；The indifferent gas
Body is selected from one of helium, neon, argon gas.
Preferably, di-iron trioxide described in step III, yttrium oxide, lanthana, titanium oxide, water, abrading-ball mass ratio be
(75-80):(1-2):(1-2):(3-5):(50-120):(180-300)。
Preferably, magnetism described in step IV inhales wave active constituent, ethyl alcohol, chloromethyl triethoxysilane, amino modified
The mass ratio of fullerene is 1:(5-10): 0.2:(0.3-0.5).
Preferably, the polyamide-based condensation polymer of ferrocenyl described in step V, cyano-thiophene class addition polymers, fullerene coat
Magnetism inhales wave active constituent, the mass ratio of metal organic frame is 1:(0.6-0.8): (0.1-0.2): 0.1.
Preferably, the metal organic frame is selected from one or more of ZIF-8, ZIF-67, MIL-101 (Fe).
Preferably, the extrusion molding, process conditions are as follows: heating temperature is 230-260 DEG C, and head extrusion temperature is 220-
240 DEG C, extruder driving screw revolving speed 110-130r/min, feed revolving speed 160-180r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
The beneficial effects of adopting the technical scheme are that
1) medical instrument absorbing material provided by the invention, preparation method is simple, and preparation cost is cheap, and raw material is easy
, it is little to device dependence.
2) medical instrument absorbing material provided by the invention, overcoming the existing wave range of inhaling of traditional absorbing material has
Limit, wave-absorbing effect need the technical issues of being further increased, with absorbing property is good, absorption band is wide, good compatibility, quality
Gently, thickness is thin, mechanical property and the advantages of Good Heat-resistance.
3) medical instrument absorbing material provided by the invention, the advantages of combining condensation polymer and addition polymers, in condensation polymer
Introduce ferrocene and thiophene-structure on molecular backbone, due to conjugation, there is certain electric conductivity, addition polymers epoxy thiophene and
Aniline structure, it is not only good with condensation polymer compatibility, but also there is positive effect to electric conductivity is improved；In addition, in addition polymers side chain
On introduce itrile group structure, improve mechanical mechanics property, stability and the weatherability of material, and the raising to material conductivity
Also there is facilitation, to it is preferred that improve wave-sucking performance.
4) medical instrument absorbing material provided by the invention introduces fullerene coated magnetic and inhales wave active constituent, a side
Face is conducive to the raising of inorganic matter Yu organic matter compatibility, so that inorganic matter dispersion is more uniform, on the other hand, is conducive to material
Material carries out humidification, improves mechanical property, furthermore, synergistic effect improves wave-sucking performance；Metal organic frame is introduced, it is utilized
Cavity structure plays the role of certain suction wave；Each ingredient synergistic effect improves material mechanical performance and inhales wave and inhales wave range and suction
Wave effect.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, and make features described above of the invention,
Purpose and advantage are more clear understandable, and the present invention will be further explained with reference to the examples below.Embodiment is only used for
It is bright the present invention rather than limit the scope of the invention.
Present invention raw material as used in the following examples is purchased from upper Haiquan sunrise foreign trade Co., Ltd.
Embodiment 1
A kind of preparation method of medical instrument absorbing material, includes the following steps:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: by 1,1- diamino ferrocene 12.5g, 2,5- thiophene dicarboxylic acid
10g is added in dimethyl sulfoxide 80g, and lower 150 DEG C of normal pressure are reacted 1 hour, then 1- ethyl-(3- dimethylamino third is added thereto
Base) carbodiimide hydrochloride 4g, 4-dimethylaminopyridine 2g, 210 DEG C are warming up to, primary polycondensate reacts 5 hours, then will reaction
Liquid is transferred in reaction kettle, vacuumizes (500Pa), is heated to 240 DEG C, then polycondensation reaction 8 hours, after be precipitated in water, will be precipitated
Polymer washed 3 times with acetone, then rotate removing acetone, obtain the polyamide-based condensation polymer of ferrocenyl；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile 10g, 4- amino two
Styrene 10g, azodiisobutyronitrile 0.1g are dissolved in N-Methyl pyrrolidone 80g, and it is small to be stirred to react 4 at 70 DEG C of nitrogen atmosphere
When, after be precipitated in water, and by the addition polymers of precipitation with ethanol washing 3 times, then to be placed at 80 DEG C of vacuum oven dry 10 small
When, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: di-iron trioxide 75g, yttrium oxide 1g, lanthana 1g, titanium oxide 3g are mixed
Conjunction obtains mixture, then is added to water 50g and abrading-ball 180g to mixture, carries out wet grinding 8 hours, does at 110 DEG C
It is dry processing 2 hours, after be orientated in the magnetic field of 6000A/m, after the pressure compression moulding of 18MPa, place into Muffle furnace into
Row sintering, sintering temperature are 1000 DEG C, with room temperature is furnace-cooled to after heat preservation 3 hours, obtain magnetism and inhale wave active constituent；
IV fullerene coated magnetic inhales wave active constituent: the magnetic suction wave active constituent that will be prepared by step III
10g is scattered in ethyl alcohol 50g, after chloromethyl triethoxysilane 2g is added thereto, be stirred to react at 60 DEG C 4 hours, after
Amino modified fullerene 3g is added thereto again, continues to be stirred to react 6 hours, then filter, be washed 3 times with ethyl alcohol, then be placed in vacuum
It is 10 hours dry at 80 DEG C in drying box, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer 10g of ferrocenyl being prepared by step I, pass through
Cyano-thiophene class addition polymers 6g that step II is prepared, wave activity is inhaled by the fullerene coated magnetic that step IV is prepared
Ingredient 1g, metal organic frame ZIF-81g are added in high-speed mixer, and high speed dispersion is squeezed by extrusion shaping machine after twenty minutes
It forms out and absorbing material is made；The extrusion molding, process conditions are as follows: heating temperature is 230 DEG C, and head extrusion temperature is 220
DEG C, extruder driving screw revolving speed 110r/min, feed revolving speed 160r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
Embodiment 2
A kind of preparation method of medical instrument absorbing material, includes the following steps:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: by 1,1- diamino ferrocene 12.5g, 2,5- thiophene dicarboxylic acid
10g is added in n,N-Dimethylformamide 90g, and lower 155 DEG C of normal pressure are reacted 1.2 hours, then 1- ethyl-(3- bis- is added thereto
Dimethylaminopropyl) carbodiimide hydrochloride 4.5g, 4-dimethylaminopyridine 2.3g, 215 DEG C are warming up to, primary polycondensate reaction
5.5 hours, then reaction solution is transferred in reaction kettle, vacuumizes (500Pa), is heated to 243 DEG C, then polycondensation reaction 8.5 hours,
It is precipitated in water afterwards, the polymer of precipitation is washed 4 times, then rotate removing acetone with acetone, obtain the polyamide-based contracting of ferrocenyl
Polymers；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile 10g, 4- amino two
Styrene 10g, azobisisoheptonitrile 0.13g are dissolved in N-Methyl pyrrolidone 90g, are stirred to react at 72 DEG C of helium atmosphere
4.5 hours, after be precipitated in water, and by the addition polymers of precipitation with ethanol washing 4 times, then be placed at 83 DEG C of vacuum oven dry
12 hours, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: by di-iron trioxide 77g, yttrium oxide 1.3g, lanthana 1.2g, titanium oxide
3.5g is mixed to get mixture, then is added to water 65g and abrading-ball 200g to mixture, carries out wet grinding 8.5 hours, then at
Be dried 2.5 hours at 113 DEG C, after be orientated in the magnetic field of 7000A/m, after the pressure compression moulding of 20Mpa, place into
Be sintered in Muffle furnace, sintering temperature is 1050 DEG C, with room temperature is furnace-cooled to after heat preservation 4 hours, obtain it is magnetic inhale wave activity at
Point；
IV fullerene coated magnetic inhales wave active constituent: the magnetic suction wave active constituent that will be prepared by step III
10g is scattered in ethyl alcohol 65g, after chloromethyl triethoxysilane 2g is added thereto, be stirred to react at 65 DEG C 4.5 hours,
Amino modified fullerene 3.5g is added thereto again afterwards, continues to be stirred to react 6.5 hours, then filter, be washed 4 times with ethyl alcohol, then set
It is 12 hours dry at 84 DEG C in a vacuum drying oven, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer 10g of ferrocenyl being prepared by step I, pass through
Cyano-thiophene class addition polymers 6.5g that step II is prepared, to inhale wave by the fullerene coated magnetic that step IV is prepared living
Property ingredient 1.4g, metal organic frame ZIF-671g be added in high-speed mixer, by being extruded into after high speed dispersion 25 minutes
Absorbing material is made in type machine extrusion molding；The extrusion molding, process conditions are as follows: heating temperature is 235 DEG C, head extrusion temperature
It is 225 DEG C, extruder driving screw revolving speed 115r/min, feed revolving speed 165r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
Embodiment 3
A kind of preparation method of medical instrument absorbing material, includes the following steps:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: by 1,1- diamino ferrocene 12.5g, 2,5- thiophene dicarboxylic acid
10g is added in N-Methyl pyrrolidone 100g, and lower 160 DEG C of normal pressure are reacted 1.5 hours, then 1- ethyl-(3- diformazan is added thereto
Base aminopropyl) carbodiimide hydrochloride 5g, 4-dimethylaminopyridine 2.5g, 220 DEG C are warming up to, primary polycondensate reacts 6 hours,
Then reaction solution is transferred in reaction kettle, vacuumizes (500Pa), be heated to 246 DEG C, then polycondensation reaction 9 hours, after analyse in water
Out, the polymer of precipitation is washed 5 times with acetone, then rotates removing acetone, obtain the polyamide-based condensation polymer of ferrocenyl；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile 10g, 4- amino two
Styrene 10g, azodiisobutyronitrile 0.15g are dissolved in N-Methyl pyrrolidone 100g, are stirred to react 5 at 76 DEG C of neon atmosphere
Hour, after be precipitated in water, and by the addition polymers of precipitation with ethanol washing 5 times, then be placed at 86 DEG C of vacuum oven dry
13.5 hours, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: by di-iron trioxide 78g, yttrium oxide 1.6g, lanthana 1.5g, titanium oxide
4g is mixed to get mixture, then is added to water 100g and abrading-ball 230g to mixture, carries out wet grinding 9 hours, then at 116 DEG C
It is lower be dried 3 hours, after be orientated in the magnetic field of 7500A/m, after the pressure compression moulding of 21Mpa, place into Muffle furnace
In be sintered, sintering temperature is 1100 DEG C, with room temperature is furnace-cooled to after heat preservation 5 hours, obtains magnetic inhaling wave active constituent；
IV fullerene coated magnetic inhales wave active constituent: the magnetic suction wave active constituent that will be prepared by step III
10g is scattered in ethyl alcohol 80g, after chloromethyl triethoxysilane 2g is added thereto, be stirred to react at 70 DEG C 5 hours, after
Amino modified fullerene 4g is added thereto again, continues to be stirred to react 7 hours, then filter, be washed 5 times with ethyl alcohol, then be placed in vacuum
It is 14 hours dry at 86 DEG C in drying box, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer 10g of ferrocenyl being prepared by step I, pass through
Cyano-thiophene class addition polymers 7.2g that step II is prepared, to inhale wave by the fullerene coated magnetic that step IV is prepared living
Property ingredient 1.7g, metal organic frame MIL-101 (Fe) 1g be added in high-speed mixer, by squeezing after high speed dispersion 30 minutes
Absorbing material is made in molding machine extrusion molding out；The extrusion molding, process conditions are as follows: heating temperature is 245 DEG C, head extrusion
Temperature is 230 DEG C, extruder driving screw revolving speed 120r/min, and feed revolving speed 170r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
Embodiment 4
A kind of preparation method of medical instrument absorbing material, includes the following steps:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: by 1,1- diamino ferrocene 12.5g, 2,5- thiophene dicarboxylic acid
10g is added in high boiling solvent 110g, and lower 165 DEG C of normal pressure are reacted 1.8 hours, then 1- ethyl-(3- dimethylamino is added thereto
Base propyl) carbodiimide hydrochloride 5.5g, 4-dimethylaminopyridine 2.8g, 225 DEG C are warming up to, primary polycondensate reacts 6.5 hours,
Then reaction solution is transferred in reaction kettle, vacuumizes (500Pa), be heated to 248 DEG C, then polycondensation reaction 9.5 hours, after in water
It is precipitated, the polymer of precipitation is washed 4 times, then rotate removing acetone with acetone, obtain the polyamide-based condensation polymer of ferrocenyl；It is described
It is mixed that high boiling solvent is that dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone 1:2:1 in mass ratio are mixed
Close object；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile 10g, 4- amino two
Styrene 10g, initiator 0.18g are dissolved in N-Methyl pyrrolidone 115g, and it is small to be stirred to react 5.5 at 78 DEG C of argon atmosphere
When, after be precipitated in water, and by the addition polymers of precipitation with ethanol washing 4 times, then be placed at 89 DEG C of vacuum oven dry 14.5
Hour, obtain cyano-thiophene class addition polymers；The initiator is azodiisobutyronitrile, azobisisoheptonitrile 3:5 in mass ratio mixed
Mixture made of conjunction；
The III magnetic preparation for inhaling wave active constituent: by di-iron trioxide 78g, yttrium oxide 1.8g, lanthana 1.9g, titanium oxide
4.7g is mixed to get mixture, then is added to water 115g and abrading-ball 280g to mixture, carries out wet grinding 9.5 hours, then at
Be dried 3.8 hours at 118 DEG C, after be orientated in the magnetic field of 8500A/m, after the pressure compression moulding of 22Mpa, place into
It is sintered in Muffle furnace, sintering temperature is 1200 DEG C, with room temperature is furnace-cooled to after heat preservation 5.5 hours, obtains magnetic suction wave activity
Ingredient；
IV fullerene coated magnetic inhales wave active constituent: the magnetic suction wave active constituent that will be prepared by step III
10g is scattered in alcohol 95 g, after chloromethyl triethoxysilane 2g is added thereto, be stirred to react at 78 DEG C 5.5 hours,
Amino modified fullerene 4.7g is added thereto again afterwards, continues to be stirred to react 7.8 hours, then filter, be washed 5 times with ethyl alcohol, then set
It is 14.5 hours dry at 88 DEG C in a vacuum drying oven, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer 10g of ferrocenyl being prepared by step I, pass through
Cyano-thiophene class addition polymers 7.9g that step II is prepared, to inhale wave by the fullerene coated magnetic that step IV is prepared living
Property ingredient 2g, metal organic frame 1g be added in high-speed mixer, pass through extrusion shaping machine after high speed dispersion 37 minutes and squeeze out
It forms and absorbing material is made；The metal organic frame is ZIF-8, ZIF-67, MIL-101 (Fe) 1:2:1 in mass ratio mixing
Made of mixture；The extrusion molding, process conditions are as follows: heating temperature is 255 DEG C, and head extrusion temperature is 235 DEG C, is squeezed out
Owner screw speed 125r/min, feed revolving speed 175r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
Embodiment 5
A kind of preparation method of medical instrument absorbing material, includes the following steps:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: by 1,1- diamino ferrocene 12.5g, 2,5- thiophene dicarboxylic acid
10g is added in dimethyl sulfoxide 120g, and lower 170 DEG C of normal pressure are reacted 2 hours, then 1- ethyl-(3- dimethylamino third is added thereto
Base) carbodiimide hydrochloride 6g, 4-dimethylaminopyridine 3g, 230 DEG C are warming up to, primary polycondensate reacts 7 hours, then will reaction
Liquid is transferred in reaction kettle, vacuumizes (500Pa), is heated to 250 DEG C, then polycondensation reaction 10 hours, after be precipitated in water, will be precipitated
Polymer washed 5 times with acetone, then rotate removing acetone, obtain the polyamide-based condensation polymer of ferrocenyl；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile 10g, 4- amino two
Styrene 10g, azobisisoheptonitrile 0.2g are dissolved in N-Methyl pyrrolidone 120g, are stirred to react 6 at 80 DEG C of nitrogen atmosphere
Hour, after be precipitated in water, and by the addition polymers of precipitation with ethanol washing 5 times, then be placed at 90 DEG C of vacuum oven dry 15
Hour, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: di-iron trioxide 80g, yttrium oxide 2g, lanthana 2g, titanium oxide 5g are mixed
Conjunction obtains mixture, then is added to water 120g and abrading-ball 300g to mixture, carries out wet grinding 10 hours, at 120 DEG C
Be dried 4 hours, after be orientated in the magnetic field of 9000A/m, after the pressure compression moulding of 23Mpa, place into Muffle furnace
It is sintered, sintering temperature is 1200 DEG C, with room temperature is furnace-cooled to after heat preservation 6 hours, obtains magnetic suction wave active constituent；
IV fullerene coated magnetic inhales wave active constituent: the magnetic suction wave active constituent that will be prepared by step III
10g is scattered in ethyl alcohol 100g, after chloromethyl triethoxysilane 2g is added thereto, be stirred to react at 80 DEG C 6 hours, after
Amino modified fullerene 5g is added thereto again, continues to be stirred to react 8 hours, then filter, be washed 5 times with ethyl alcohol, then be placed in vacuum
It is 15 hours dry at 90 DEG C in drying box, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer 10g of ferrocenyl being prepared by step I, pass through
Cyano-thiophene class addition polymers 8g that step II is prepared, wave activity is inhaled by the fullerene coated magnetic that step IV is prepared
Ingredient 2g, metal organic frame MIL-101 (Fe) 1g are added in high-speed mixer, and high speed dispersion passes through after forty minutes to be extruded into
Absorbing material is made in type machine extrusion molding；The extrusion molding, process conditions are as follows: heating temperature is 260 DEG C, head extrusion temperature
It is 240 DEG C, extruder driving screw revolving speed 130r/min, feed revolving speed 180r/min.
A kind of medical instrument absorbing material is prepared using the preparation method of above-mentioned medical instrument absorbing material.
A kind of medical instrument uses absorbing material as sheathing material using above-mentioned medical instrument.
Comparative example
A kind of medical instrument absorbing material, according to 201711359454.8 embodiment 1 of Chinese invention patent formula and
Preparation method is prepared.
The absorbing material described in above-described embodiment 1-5 and comparative example is tested for the property, test result and test method
It is shown in Table 1.
Table 1
| Performance | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example | Detection method |
| Limit oxygen index (%) | 37 | 39 | 40 | 42 | 45 | 28 | GB/T2406-1993 |
| Tensile strength (MPa) | 43 | 45 | 46 | 48 | 50 | 40 | GB/T1040.1-2006 |
| Bending modulus (MPa) | 2720 | 2725 | 2730 | 2736 | 2740 | 2700 | GB1042-79 |
| Simply supported beam notch shock (KJ/m2) | 7.5 | 7.7 | 8.0 | 8.2 | 8.5 | 7.2 | GB1043-79 |
| Maximum reflectivity (dB) | -26 | -28 | -29 | -30 | -30 | -20 | GJB 5239-2004 |
As seen from Table 1, medical instrument absorbing material disclosed by the embodiments of the present invention, with absorbing material in the prior art
It compares, there is more excellent anti-flammability, mechanical property and wave-sucking performance.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of preparation method of medical instrument absorbing material, which comprises the steps of:
The preparation of the polyamide-based condensation polymer of I ferrocenyl: higher boiling is added in 1,1- diamino ferrocene, 2,5- thiophene dicarboxylic acid
In solvent, 150-170 DEG C reaction 1-2 hours under normal pressure, then two Asia of 1- ethyl-(3- dimethylaminopropyl) carbon is added thereto
Amine hydrochlorate, 4-dimethylaminopyridine are warming up to 210-230 DEG C, and primary polycondensate reacts 5-7 hours, is then transferred to reaction solution
In reaction kettle, vacuumize (500Pa), be heated to 240-250 DEG C, then polycondensation reaction 8-10 hours, after be precipitated in water, will be precipitated
Polymer washed 3-5 times with acetone, then rotate removing acetone, obtain the polyamide-based condensation polymer of ferrocenyl；
The preparation of II cyano-thiophene class addition polymers: by (2- thenylidene) methane -1,1'- dimethoxy nitrile, 4- amino-stilbene,
Initiator is dissolved in N-Methyl pyrrolidone, is stirred to react at nitrogen or 70-80 DEG C of atmosphere of inert gases 4-6 hours, after
It is precipitated in water, and by the addition polymers of precipitation with ethanol washing 3-5 times, then to be placed at 80-90 DEG C of vacuum oven dry 10-15 small
When, obtain cyano-thiophene class addition polymers；
The III magnetic preparation for inhaling wave active constituent: being mixed to get mixture for di-iron trioxide, yttrium oxide, lanthana, titanium oxide,
It is added to water and abrading-ball to mixture again, carries out wet grinding 8-10 hours, is dried 2-4 hours at 110-120 DEG C,
It is orientated in the magnetic field of 6000-9000A/m afterwards, after the pressure compression moulding of 18MPa-23Mpa, places into Muffle furnace and carry out
Sintering, sintering temperature are 1000-1200 DEG C, with room temperature is furnace-cooled to after heat preservation 3-6 hours, obtain magnetic suction wave active constituent；
IV fullerene coated magnetic inhales wave active constituent: dispersing the magnetic wave active constituent of inhaling being prepared by step III in
In ethyl alcohol, after chloromethyl triethoxysilane is added thereto, be stirred to react at 60-80 DEG C 4-6 hours, after again thereto plus
Enter amino modified fullerene, continues to be stirred to react 6-8 hours, then filter, be washed 3-5 times with ethyl alcohol, then be placed in a vacuum drying oven
It is 10-15 hours dry at 80-90 DEG C, it obtains fullerene coated magnetic and inhales wave active constituent；
The preparation of V absorbing material: by the polyamide-based condensation polymer of ferrocenyl being prepared by step I, by step II system
Standby obtained cyano-thiophene class addition polymers inhale wave active constituent, metal by the fullerene coated magnetic that step IV is prepared
Organic frame is added in high-speed mixer, is made after high speed dispersion 20-40 minutes by extrusion shaping machine extrusion molding and is inhaled wave
Material.
2. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described in step I
1,1- diamino ferrocene, 2,5- thiophene dicarboxylic acid, high boiling solvent, 1- ethyl-(3- dimethylaminopropyl) carbodiimide
Hydrochloride, 4-dimethylaminopyridine mass ratio be 1.25:1:(8-12): (0.4-0.6): (0.2-0.3)；The higher boiling is molten
Agent is selected from one or more of dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone.
3. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described in step II
(2- thenylidene) methane -1,1'- dimethoxy nitrile, 4- amino-stilbene, initiator, N-Methyl pyrrolidone mass ratio be
1:1:(0.01-0.02):(8-12)；The initiator is selected from least one of azodiisobutyronitrile, azobisisoheptonitrile；Institute
It states inert gas and is selected from one of helium, neon, argon gas.
4. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described in step III
Di-iron trioxide, yttrium oxide, lanthana, titanium oxide, water, abrading-ball mass ratio be (75-80): (1-2): (1-2): (3-5):
(50-120):(180-300)。
5. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described in step IV
Magnetism inhale wave active constituent, ethyl alcohol, chloromethyl triethoxysilane, amino modified fullerene mass ratio be 1:(5-10):
0.2:(0.3-0.5)。
6. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described in step V
The polyamide-based condensation polymer of ferrocenyl, cyano-thiophene class addition polymers, fullerene coated magnetic inhale wave active constituent, metal has machine frame
The mass ratio of frame is 1:(0.6-0.8): (0.1-0.2): 0.1.
7. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that the metal is organic
Frame is selected from one or more of ZIF-8, ZIF-67, MIL-101 (Fe).
8. the preparation method of medical instrument absorbing material according to claim 1, which is characterized in that described to be extruded into
Type, process conditions are as follows: heating temperature is 230-260 DEG C, and head extrusion temperature is 220-240 DEG C, extruder driving screw revolving speed
110-130r/min, feed revolving speed 160-180r/min.
9. a kind of medical treatment that the preparation method using any one of claim 1-8 medical instrument absorbing material is prepared
Instrument absorbing material.
10. a kind of use absorbing material as the medical instrument of sheathing material using medical instrument described in claim 9.
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