CN108559016A - A kind of amination graphene oxide bromobutyl acceptable packaging material and preparation method thereof - Google Patents
A kind of amination graphene oxide bromobutyl acceptable packaging material and preparation method thereof Download PDFInfo
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- CN108559016A CN108559016A CN201810535859.0A CN201810535859A CN108559016A CN 108559016 A CN108559016 A CN 108559016A CN 201810535859 A CN201810535859 A CN 201810535859A CN 108559016 A CN108559016 A CN 108559016A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/08—Butenes
- C08F210/10—Isobutene
- C08F210/12—Isobutene with conjugated diolefins, e.g. butyl rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
- C08F8/22—Halogenation by reaction with free halogens
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2800/00—Copolymer characterised by the proportions of the comonomers expressed
- C08F2800/20—Copolymer characterised by the proportions of the comonomers expressed as weight or mass percentages
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Abstract
The invention discloses a kind of amination graphene oxide bromobutyl acceptable packaging materials, graphene oxide is carried out first amination modified, amination graphene oxide butyl rubber is obtained by the reaction with butyl rubber monomer mixture later, through solwution method bromination, washing is neutralized, the post-processing of BIIR can be obtained amination graphene oxide bromobutyl acceptable packaging material later.The amination graphene oxide bromobutyl acceptable packaging material that this method is prepared has excellent anti-microbial property, and intensity is high, and elasticity is good, and material homogeneity is good, and puncture is not easy furfur.
Description
Technical field
The present invention relates to medical packaging Material Field more particularly to a kind of graphene bromobutyl acceptable packaging material and
Preparation method.
Background technology
Drug is a kind of special commodity, due to by illumination, humidity, microbial contamination isoperimetric collarette in the process of circulation
The influence in border is easy to decomposed metamorphic, after drug machine-shaping, it is necessary to select suitable packaging that could keep the effect of drug
Energy the stability for keeping drug, delays drug to go bad, ensures the drug safety of broad masses of the people, therefore, pharmaceutical packing quilt
Referred to as " the second life " of drug.Qualified Key works Drug packing should have that sealing, stabilization, light, beautiful, specification is suitable, packaging mark
Know specification, it is reasonable, clear the features such as, also meet drug flow, storage firmly, using the requirement of each link.
With the development of society, the rubber product type applied to medicine and hygiene fields is more and more, such as various flask for medicinal preparations
Rubber plug, asepsis injector piston, syringe sealant sealing, hose, conduit, medical air cushion, antiseptic rubber medical gloves, baby
Youngster's nipple, tube for blood transfusion,latex etc..Ideal druggist rubber sundrier does not need only to have good physical property, it is necessary to ensure nontoxic
And have chemical inertness, especially internal rubber product should have it is not pathogenic, do not damage adjacent tissue, do not cause allergy, aging
The features such as performance is good.
Traditional medical, medicinal rubber product under high temperature, condition of high voltage, vulcanizing system easy to produce pollution human body,
Exudate, the volatile matter of medicament, to be difficult to prepare medical, the medicinal rubber product that meet drug best quality standard.It is existing
Medical, medicinal rubber product and preparation method thereof, complex technical process, the product feature of environmental protection is poor, and safety in utilization is low, and makes
It is shorter with the service life.
Brombutyl（BIIR）It is butyl rubber（IIR）A kind of halogenated products, it had both had butyl rubber in gas
The advantages of close property, heat resistance, ageing resistance, corrosion resistance and electrical insulating property etc., and butyl rubber is overcome in cure
The shortcomings that in terms of the processed and applieds such as energy, tack, mutual viscosity, auto industry, pharmaceuticals industry, anti-corrosion chemical defence have been widely used in it
Equal fields.But the chlorinated butyl rubber bung as medical rubber plug, in processing synthesizes, the additive amount of certain reinforcing agents is difficult to control
System, frequently can lead to the unstable of rubber plug physical property, especially in terms of puncturing exfoliation, increases the dangerous row of medication,
Therefore the bromobutyl medicinal materials that active development intensity is high, non-toxic, stability is good, anti-microbial property is good are needed.
Graphene（Graphene）It is a kind of two dimension that hexagon being formed in honeycomb lattice with sp2 hybridized orbits by carbon atom
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine
It is with important application prospects with drug delivery etc., it is considered to be a kind of future revolutionary material.As a kind of uniqueness
Monoatomic layer two-dimensional structure material, high carrier mobility, thermal coefficient, specific surface area, light transmittance and excellent mechanics
Performance becomes a kind of ideal carbon material for preparing polymer nanocomposites.The Young's modulus of graphene can reach
1100GPa, fracture strength are up to 125GPa.Chinese invention patent CN105419129A discloses a kind of graphene-halobutyl
The preparation method of rubber composite material, including：Surfactant is added in graphene oxide dispersion, function is obtained by the reaction
Change graphene oxide dispersion, reducing agent is added to cleaning after being reacted in functional graphene oxide dispersion liquid, work(is obtained by filtration
Energy graphite alkene precipitation, functionalization graphene precipitation is scattered in organic solvent and obtains functionalization graphene dispersion liquid, by work(
Energy graphite alkene dispersion liquid is uniformly mixed to obtain graphene-halogenated butyl rubber suspension with halogenated butyl rubber latex, suspends
Graphene-halogenated butyl rubber composite material is obtained after liquid solidification.This method is in preparation process, halogenated butyl rubber and function
In graphite alkene recombination process, halogenated butyl rubber easy tos produce agglomeration, and obtained composite material homogeneity is poor, and gained
The anti-microbial property of product is to be improved.Seek that a kind of anti-microbial property is good, material homogeneity is good, intensity is high and elasticity is good, punctures not
The bromobutyl acceptable packaging material of furfur is current development trend.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of amination graphene oxide bromines
The preparation method of butyl rubber acceptable packaging material overcomes the anti-microbial property of bromobutyl acceptable packaging material in the prior art
Difference, material homogeneity are poor, and intensity is low, poor flexibility, punctures the technical problems such as easy furfur.
To achieve the goals above or other purposes, the present invention is achieved by the following technical solutions：
A kind of preparation method of amination graphene oxide bromobutyl acceptable packaging material, which is characterized in that include mainly
Following steps：
（1）By graphene oxide amination, amination graphene oxide is obtained；
（2）Chloromethanes, butyl rubber monomer mixture are added to step（1）Obtained amination graphene oxide organic solvent
In dispersion liquid；Amination graphene oxide butyl rubber glue is prepared using solwution method；
（3）Using solwution method by step（2）Obtained amination graphene oxide butyl rubber glue bromination, it is neutralized washing and
Finished product amination graphene oxide bromobutyl acceptable packaging material is obtained after the post-processing of BIIR.
A kind of preparation method of amination graphene oxide bromobutyl acceptable packaging material, which is characterized in that including
Following steps：
（1）Make graphene oxide and reacting ethylenediamine, amination graphene oxide is prepared；
（2）By step（1）Obtained amination graphene oxide is scattered in organic solvent, obtains the amination oxygen of 1-15g/L
Graphite alkene dispersion liquid, the monomer mixture of chloromethanes and butyl rubber is added in amination graphene oxide dispersion,
It is reacted 5-10 hours using solwution method, obtains amination graphene oxide butyl rubber glue；
（3）Using solwution method by step（2）Obtained amination graphene oxide butyl rubber glue and active bromine reaction, in
Finished product amination graphene oxide bromobutyl acceptable packaging material is obtained with after washing and the post-processing of BIIR.
Further, step（1）In, ethylenediamine and graphene oxide are added in organic solvent, are warming up to 60-65 DEG C
Back flow reaction obtains amination graphene oxide.
Preferably, step（1）In, graphene oxide is scattered in dimethylformamide at 30 DEG C, be ultrasonically treated and
Mechanical agitation 1 hour forms graphene oxide dispersion, ethylenediamine is added in dispersion liquid later, is ultrasonically treated and mechanical
Stirring 1 hour is added coupling agent HATU, and mixture is transferred in 60 DEG C -65 DEG C of water-bath later, be carried out at the same time stirring and
Reflux condensation mode 6 hours, obtains amination graphene oxide.
Further, the quality parts ratio that feeds intake of ethylenediamine and graphene oxide is（2-3）：1.
Preferably, the quality parts ratio that feeds intake of ethylenediamine and graphene oxide is 2：1.
Further, the graphene oxide grain size is 10-1000nm.
Preferably, the graphene oxide grain size is 100-500nm.
Most preferably, the graphene oxide grain size is 200-300nm.
Further, step（2）The monomer mixture of the bromobutyl includes isoalkene and polyene.Wherein, institute
Stating isoalkene preferably has 4 to 16 carbon atoms, more preferable 4-7 carbon atom, such as isobutene, 2-methyl-1-butene alkene, 3- first
Base -1- butylene, 2- methyl-2-butenes, 4-methyl-1-pentene and its mixture.Most preferably isobutene.
Each polyene well known by persons skilled in the art, can be copolymerized with isoalkene can be used in the polyene.It is preferred that
Polyene with 4-14 carbon atom, as between isoprene, butadiene, 2-methyl butadiene, 2,4- dimethyl butadienes, penta
Diene, 3- methyl-1,3-pentylenes, 2,4- hexadienes, 2- neopentyls butadiene, 2- methyl-1s, 5- hexadienes, 2,5- diformazans
Base -2,4- hexadienes, 2- methyl-1s, 4- pentadienes, 2- methyl-1s, 6- heptadiene, cyclopentadiene, methyl cyclopentadiene, hexamethylene
Diene, 1- vinyl cyclohex diene and its mixture, especially conjugated diene.
Most preferably isoprene.
Further, the monomer mixture of the butyl rubber preferably includes at least one isoolefin monomer of 80-100%
With at least one multi-olefin monomer of 0-20%.
Further, the butyl rubber monomer mixture includes the isoalkene of 96%-99.75% and the polyenoid of 0.25%-4%
Hydrocarbon.
Further, the butyl rubber monomer mixture is isobutene and isoprene, wherein isobutene and isoamyl
The mass percent of diene is respectively 96%-99.75% and 0.25%-4%.
Further, step（2）Described in butyl rubber monomer mixture and amination graphene oxide the quality that feeds intake
Portion rate is（80-100）:1.
Further, step（2）Described in organic solvent be non-polar organic solvent, selected from n-hexane, carbon tetrachloride, chlorine
Imitative, hexamethylene, butane, iso-butane, pentane, isopentane, neopentane, isohexane, 3- methylpentanes, neohexane, 2,3- diformazans
One or more of base butane, normal heptane, benzene, toluene.Preferably, step（2）Described in organic solvent be n-hexane.
Further, which is characterized in that step（3）Middle active bromine is selected from sulfonic acid bromide, bis- bromo- 5,5- dimethyl of 1,3- in oneself
Uride iodobenzene bromine, bromine, bromine chloride, sodium hypobromite, sulfur bromide, N- bromination succinimines, the active bromine are aoxidized with amination
The weight part ratio of graphene butyl rubber is（2-2.5）：1.
Preferably, the active bromine is bromine.
The present invention also provides amination graphene oxide butyl rubber acceptable packaging materials made from method made above.
The present invention also provides the amination graphene oxide butyl rubber acceptable packaging material of gained is medicinal in injection
The application of rubber plug etc..
In summary, the present invention has the following technical effect that：
（1）The present invention provides a kind of bromobutyl of amidized graphene oxide modification, amination graphene oxide materials
The addition of material makes obtained bromobutyl intensity improve, and more preferably, bits are not fallen in nontoxic and puncture to stability, and with excellent
Good anti-microbial property.
（2）The present invention also provides a kind of preparation sides of amination graphene oxide bromobutyl acceptable packaging material
Graphene oxide is first carried out amination by method, this method, so that the carbonyl in its graphene oxide structure is grafted with ethylenediamine, later
The butyl material that Uniform Doped amination graphene oxide is obtained by the reaction in butyl rubber monomer mixture is added, avoids straight
It connects and the agglomeration that rubber latex generates is added, material homogeneity is good.
（3）In the preparation method of amination graphene oxide bromobutyl acceptable packaging material provided by the invention, base
Plinth glue amination graphene oxide butyl rubber glue and bromination step are all made of solwution method, and processing step is greatly saved,
There is very high industrial application value.
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this explanations below by way of particular specific embodiment
Content disclosed by book understands other advantages and effect of the present invention easily.The present invention can also be by addition different specific
Embodiment is embodied or practiced, and the various details in this specification can also be based on different viewpoints and application, not carry on the back
Various modifications or alterations are carried out under spirit from the present invention.
It should be noted that in the absence of conflict, the feature in following embodiment and embodiment can be combined with each other.Also
It should be appreciated that the term used in the embodiment of the present invention is to describe specific specific embodiment, rather than in order to limit
Protection scope of the present invention.The test method of actual conditions is not specified in the following example, usually according to normal condition, or presses
According to the condition proposed by each manufacturer.
When embodiment provides numberical range, it should be appreciated that except non-present invention is otherwise noted, two ends of each numberical range
Any one numerical value can be selected between point and two endpoints.Unless otherwise defined, in the present invention all technologies for using and
Record of the scientific terminology with those skilled in the art to the grasp of the prior art and the present invention, can also use and this hair
Any method, equipment and the material of the similar or equivalent prior art of method, equipment described in bright embodiment, material is realized
The present invention.
Embodiment 1
The grain size 10-200nm graphene oxides of 1 mass fraction are scattered in dimethylformamide at 30 DEG C, are ultrasonically treated
With mechanical agitation 1 hour, graphene oxide dispersion is formed, the ethylenediamine of 2 mass fractions is added in dispersion liquid later, surpassed
Sonication and mechanical agitation 1 hour, are added the coupling agent HATU of 0.1 mass fraction, and mixture is transferred to 60 DEG C -65 later
DEG C water-bath in, be carried out at the same time stirring and reflux condensation mode 5 hours, obtain amination graphene oxide.
The amination graphene oxide of 1 mass fraction is scattered in hexane, the amination graphene oxide of 1g/L is obtained
The isoprene of chloromethanes, the isobutene of 64 mass fractions and 16 mass fractions is added to amination graphite oxide by dispersion liquid
In alkene dispersion liquid, a certain amount of initiator is added, methanol stopped reaction is added in polymerisation after 5 hours.The glue of synthesis is added
Enter a certain amount of hexane to be diluted, then stirred in a heated condition to remove solvent and unreacted monomer, obtains amination
Graphene oxide butyl rubber glue.
Bromination reaction：2 times of parts by weight bromines are taken to be added in the hexane solution of certain volume, under the conditions of normal pressure is protected from light
It is injected into amination graphene oxide butyl rubber lotion, is vigorously stirred, controlling reaction temperature is 50 DEG C.Reaction 5 ~
10min。
Neutralize washing：The sodium hydroxide solution that mass fraction 5% is added after being added immediately after the arrival reaction time terminates instead
It answers, continues to stir 15min.Then deionized water will be added in glue and stirs, remove impurity and ion remaining in removing glue liquid.Stop
Only stirring waits for glue stratification, and lower water is extracted out, and so on washes the pH value of the above papery glue three times close to 7, most
The additives such as calcium stearate, epoxidized soybean oil, antioxidant are added afterwards as stabilizer.
The post-processing of BIIR：Glue is injected in boiling water and evaporates solvent, rubber is condensed into solid block, is put into baking oven
The dry finished product rubber for being about 15% to water content, it is then dry at 105 DEG C on a mill, it squeezes 1 to 2 minute,
Moisture and solvent are removed, graphene bromobutyl acceptable packaging material is obtained.
Embodiment 2
1 mass fraction grain size 200 ~ 500nm graphene oxides are scattered in dimethylformamide at 30 DEG C, be ultrasonically treated and
Mechanical agitation 1 hour forms graphene oxide dispersion, the ethylenediamine of 3 mass fractions is added in dispersion liquid later, ultrasound
Processing and mechanical agitation 1 hour are added coupling agent HATU, and mixture are transferred in 60 DEG C -65 DEG C of water-bath later, simultaneously
Be stirred with reflux condensation mode 6 hours, obtain amination graphene oxide.
The amination graphene oxide of 1 mass fraction is scattered in toluene, the amination graphene oxide of 15g/L is obtained
The isoprene of chloromethanes, the isobutene of 99 mass fractions and 1 mass fraction is added to amination graphene oxide by dispersion liquid
In dispersion liquid, a certain amount of initiator is added, polymerisation is added to the water after 7 hours only reacts.The glue of synthesis is added one
Quantitative toluene is diluted, then is stirred in a heated condition to remove solvent and unreacted monomer, and amination oxidation is obtained
Graphene butyl rubber glue.
Bromination reaction：It takes 2.5 times of parts by weight bromines to be added in the hexane solution of certain volume, condition is protected from light in normal pressure
Under be injected into amination graphene oxide butyl rubber lotion, be vigorously stirred, controlling reaction temperature be 50 DEG C.Reaction 5 ~
10min。
Neutralize washing：The sodium hydroxide solution that mass fraction 5% is added after being added immediately after the arrival reaction time terminates instead
It answers, continues to stir 15min.Then deionized water will be added in glue and stirs, remove impurity and ion remaining in removing glue liquid.Stop
Only stirring waits for glue stratification, and lower water is extracted out, and so on washes the pH value of the above papery glue three times close to 7, most
The additives such as calcium stearate, epoxidized soybean oil, antioxidant are added afterwards as stabilizer.
The post-processing of BIIR：Glue is injected in boiling water and evaporates solvent, rubber is condensed into solid block, is put into baking oven
The dry finished product rubber for being about 15% to water content, it is then dry at 105 DEG C on a mill, it squeezes 1 to 2 minute,
Moisture and solvent are removed, graphene bromobutyl acceptable packaging material is obtained.
Embodiment 3
1 mass fraction grain size 800-1000nm graphene oxides are scattered in dimethylformamide at 30 DEG C, are ultrasonically treated
With mechanical agitation 1 hour, graphene oxide dispersion is formed, the ethylenediamine of 2.5 mass fractions is added in dispersion liquid later,
It is ultrasonically treated and mechanical agitation 1 hour, coupling agent HATU is added later, and mixture is transferred in 60 DEG C -65 DEG C of water-bath,
It is carried out at the same time stirring and reflux condensation mode 8 hours, obtains amination graphene oxide.
The amination graphene oxide of 1 mass fraction is scattered in hexamethylene, the amination graphite oxide of 8g/L is obtained
The isoprene of chloromethanes, 96 mass fraction isobutenes and 4 mass fractions is added to amination graphene oxide by alkene dispersion liquid
In dispersion liquid, a certain amount of initiator is added, methanol stopped reaction is added in polymerisation after 10 hours.The glue of synthesis is added
A certain amount of hexamethylene is diluted, then is stirred in a heated condition to remove solvent and unreacted monomer, and amination is obtained
Graphene oxide butyl rubber glue.
Bromination reaction：It takes 2.2 times of parts by weight bromines to be added in the hexane solution of certain volume, condition is protected from light in normal pressure
Under be injected into amination graphene oxide butyl rubber lotion, be vigorously stirred, controlling reaction temperature be 50 DEG C.Reaction 5 ~
10min。
Neutralize washing：The sodium hydroxide solution that mass fraction 5% is added after being added immediately after the arrival reaction time terminates instead
It answers, continues to stir 15min.Then deionized water will be added in glue and stirs, remove impurity and ion remaining in removing glue liquid.Stop
Only stirring waits for glue stratification, and lower water is extracted out, and so on washes the pH value of the above papery glue three times close to 7, most
The additives such as calcium stearate, epoxidized soybean oil, antioxidant are added afterwards as stabilizer.
The post-processing of BIIR：Glue is injected in boiling water and evaporates solvent, rubber is condensed into solid block, is put into baking oven
The dry finished product rubber for being about 15% to water content, it is then dry at 105 DEG C on a mill, it squeezes 1 to 2 minute,
Moisture and solvent are removed, graphene bromobutyl acceptable packaging material is obtained.
Amination graphene oxide bromobutyl provided by the invention carries out it using graphene oxide as starting material
Amination modified, the active group contained using graphene oxide carries out covalent bonding with the amino in ethylenediamine structure, later
The bromobutyl of amination graphene oxide modification, obtained material are prepared after being mixed with butyl rubber monomer using solwution method
Mechanical property significantly improves, and has certain anti-microbial property, is not easy to puncture furfur, is more conducively applied to acceptable packaging material and leads
With.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (9)
1. a kind of preparation method of amination graphene oxide bromobutyl acceptable packaging material, which is characterized in that main packet
Include following steps：
（1）By graphene oxide amination, amination graphene oxide is obtained；
（2）Chloromethanes, butyl rubber monomer mixture are added to step（1）Obtained amination graphene oxide it is organic molten
In agent dispersing liquid, amination graphene oxide butyl rubber glue is prepared using solwution method；
（3）Using solwution method by step（2）Obtained amination graphene oxide butyl rubber glue bromination, it is neutralized washing and
Finished product amination graphene oxide bromobutyl acceptable packaging material is obtained after the post-processing of BIIR.
2. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that include the following steps：
（1）Make graphene oxide and reacting ethylenediamine, amination graphene oxide is prepared；
（2）By step（1）Obtained amination graphene oxide is scattered in organic solvent, obtains the amination oxygen of 1-15g/L
Graphite alkene dispersion liquid, the monomer mixture of chloromethanes and butyl rubber is added in amination graphene oxide dispersion,
It is reacted 5-10 hours using solwution method, obtains amination graphene oxide butyl rubber glue；
（3）Using solwution method by step（2）Obtained amination graphene oxide butyl rubber glue and active bromine reaction, in
Finished product amination graphene oxide bromobutyl acceptable packaging material is obtained with after washing and the post-processing of BIIR.
3. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 2
Method, which is characterized in that the quality parts ratio that feeds intake of the ethylenediamine and graphene oxide is（2-3）：1, the reaction time 5 ~ 8 is small
When.
4. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that step（1）Described in graphene oxide grain size be 10-1000nm.
5. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that step（2）Described in the monomer mixture of butyl rubber include isoalkene and polyene.
6. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that step（2）Described in butyl rubber monomer mixture and amination graphene oxide the mass parts that feed intake
Counting ratio is（80-100）：1；Wherein, monomer mixture include 80-100% at least one isoolefin monomer and 0-20% at least
A kind of multi-olefin monomer.
7. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that step（2）Described in organic solvent be non-polar organic solvent, selected from n-hexane, carbon tetrachloride, chloroform,
Hexamethylene, butane, iso-butane, pentane, isopentane, neopentane, isohexane, 3- methylpentanes, neohexane, 2,3- dimethyl butyrates
One or more of alkane, normal heptane, benzene, toluene.
8. a kind of preparation side of amination graphene oxide bromobutyl acceptable packaging material according to claim 1
Method, which is characterized in that step（3）Described in active bromine be bromine, the active bromine and amination graphene oxide butyl rubber
The weight part ratio of glue is（2-2.5）：1.
9. the amination graphene oxide butyl rubber pharmaceutical pack material that any methods of claim 1-8 are prepared
Material.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110200825A1 (en) * | 2010-02-17 | 2011-08-18 | Baker Hughes Incorporated | Nano-coatings for articles |
| CN105111437A (en) * | 2015-09-28 | 2015-12-02 | 中国地质大学（武汉） | Functionalized graphene oxide enhanced benzoxazine-based composite resin and preparation method thereof |
| CN105419129A (en) * | 2015-12-11 | 2016-03-23 | 江苏润德医用材料有限公司 | Preparation method and application of graphene-halogenated butyl rubber composite |
| CN105777966A (en) * | 2014-12-25 | 2016-07-20 | 中国石油天然气股份有限公司 | Process for directly producing brominated butyl rubber by solution method |
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2018
- 2018-05-30 CN CN201810535859.0A patent/CN108559016A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110200825A1 (en) * | 2010-02-17 | 2011-08-18 | Baker Hughes Incorporated | Nano-coatings for articles |
| CN105777966A (en) * | 2014-12-25 | 2016-07-20 | 中国石油天然气股份有限公司 | Process for directly producing brominated butyl rubber by solution method |
| CN105111437A (en) * | 2015-09-28 | 2015-12-02 | 中国地质大学（武汉） | Functionalized graphene oxide enhanced benzoxazine-based composite resin and preparation method thereof |
| CN105419129A (en) * | 2015-12-11 | 2016-03-23 | 江苏润德医用材料有限公司 | Preparation method and application of graphene-halogenated butyl rubber composite |
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