CN105294959A - Preparation method of anti-static organic glass - Google Patents
Preparation method of anti-static organic glass Download PDFInfo
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- CN105294959A CN105294959A CN201510458349.4A CN201510458349A CN105294959A CN 105294959 A CN105294959 A CN 105294959A CN 201510458349 A CN201510458349 A CN 201510458349A CN 105294959 A CN105294959 A CN 105294959A
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Abstract
The invention provides a preparation method of anti-static organic glass, relates to the field of preparation of anti-static function materials, and aims to solve the technical problem that the conventional organic glass is low in anti-static performance. The preparation method comprises the following steps: firstly, oxidized graphene is modified by acrylic acid or glycidyl acrylate, then the modified oxidized graphene is dispersed in a mixture of methyl methacrylate monomer and an auxiliary, and initiated polymerization is carried out through azo compounds or peroxide, so that the conductive organic glass is prepared. According to the preparation method of the anti-static organic glass, provided by the invention, the surface resistance of the anti-static organic glass membrane is 10<6>-10<10> Q, a stable anti-static function is achieved, excellent surface hardness and anti-erosion capability for chemical solvents are further achieved, the anti-static function is not influenced by humidity and temperature, the light transmittance is high, and the processing property is excellent, therefore the anti-static organic glass can be used in the field of anti-static or electromagnetic shielding materials.
Description
Technical field
The present invention relates to the preparation method of anti-static function material.
Background technology
Synthetic glass, is abbreviated as: PMMA(Polymethylmethacrylate), chemical name, polymethylmethacrylate, is the macromolecular compound become by methacrylate.Smooth surface, beautiful in colour, proportion is little, and intensity is comparatively large, and corrosion-resistant, moisture-proof, sun-proof, good insulation preformance, sound insulation property is good.Tubular material, clavate material, plate shape material three kinds can be divided.PMMA is that the polymkeric substance obtained with acrylicacidandesters Type of Collective is referred to as acrylics, polyacrylic plastics is referred to as by corresponding plastics, wherein most widely used general with polymethyl ester methyl ester, polymethylmethacrylate (PMMA) exists owing to there being huge side base, for amorphous solid, have heigh clarity, proportion is little, having certain impact strength and good low-temperature performance, is the important source material of aircraft industry and opticinstrument process industry.There is good electrical insulation capability, chemical stability and ageing resistance, higher physical strength and good moisture resistant performance is had under normal temperature, and quality is light, be easy to processing, transmittance is high, is therefore widely applied in instrument, Meter Parts, auto parts machinery, handicraft, electrical apparatus insulation material and building and ornament materials etc.But because its good electrical insulation capability is also with the problem of serving to some application aspect, namely process, transport and application process in due to other objects friction or peel off time, can produce accumulation of static electricity at material surface, this accumulation of static electricity can cause dust suction, affects material appearance.If be used as the screen of household electrical appliance as video player etc., producing accumulation of static electricity also can affect electric property.Therefore how to weaken or eliminate the accumulation of static electricity of this material surface and to prevent material surface from producing electrostatic be hot issue in macromolecular material research field always.At present macromolecular material is carried out that the method for antistatic treatment is the most frequently used and effective method uses static inhibitor to reduce the surface resistivity of material.
Graphene (Graphene) is a kind of novel material of the individual layer sheet structure be made up of carbon atom.Be a kind of by carbon atom with sp
2hybridized orbital composition hexangle type is the flat film of honeycomb lattice, only has the two-dimensional material of a carbon atom thickness.Graphene is considered to hypothetical structure always, cannot stable existence separately, until 2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, successfully from graphite, isolate Graphene in an experiment, and confirming that it can Individual existence, two people, also because of " testing in the initiative of two-dimensional graphene material ", obtain 2010 years Nobel Prizes in physics jointly.
Graphene is thin, the hardest nano material in known world, and it is almost completely transparent, only absorbs the light of 2.3%; Thermal conductivity is up to 5300W/mK, and higher than carbon nanotube and diamond, under normal temperature, its electronic mobility is more than 15000cm
2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height, and resistivity only about 10
-6Ω cm, than copper or silver lower, be the material that world resistivity is minimum.Because its resistivity is extremely low, the speed of electronic migration is exceedingly fast, and is therefore expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster.Because Graphene is in fact a kind of transparent, good conductor, be also applicable to for preparation conduction or anti-static composite material, the present invention it can be used as anti-electrostatic component to prepare anti-electrostatic synthetic glass.
Summary of the invention
The present invention seeks to the technical problem that antistatic property in order to solve existing synthetic glass is lower, and propose a kind of preparation method of Graphene modification antistatic organic glass.The present invention carries out mass polymerization by modified for Graphene with methacrylic ester methyl ester (MMA), produces anti-electrostatic poly (methyl methacrylate) plate.
In the mass polymerization of methyl methacrylate (MMA), produce gas due to heating and can only obtain alveolate polymkeric substance.If select other polymerization process (as: suspension polymerization etc.) due to the introducing of impurity, the transparency of product is all far away from bulk polymerization.In order to solve heat radiation when therefore carrying out mass polymerization with MMA, avoid Auto-acceleration and the implode phenomenon caused, and conversion of monomer when being polymkeric substance due to volumetric shrinkage problem that proportion difference causes, industrial or laboratory at present more adopts High Temperature Pre polymerization, pre-polymerization to the thick slurry of about 10% transformation efficiency, prepolymer) after, then be injected in mould, slowly polymerization makes transformation efficiency reach 93 ~ 95% at low temperatures, finally at 100 DEG C high temperature polymerization to reacting completely.Ride out critical days, finally demould obtains synthetic glass flat board, so the present invention is after Graphene is carried out functional modification, then with methyl methacrylate copolymer, adopt the teeming practice of segmentation controllable polymerization to prepare anti-electrostatic synthetic glass.Concrete summary of the invention is as follows:
1. the preparation method of a kind of anti-electrostatic synthetic glass of the present invention carries out according to the following steps:
Step one: prepared by functionalized graphite's alkene
By in graphene oxide or graphene dispersion to the body or its good solvent of acrylic or methacrylic acid glycidyl ester, under the protection of nitrogen and stopper, linked reaction 1-15 hour is carried out under the effect of 30-150 DEG C and catalyzer, remove desolventizing and residual monomer through centrifugation or underpressure distillation, then obtain functionalized graphite's alkene through repeatedly alkali cleaning, washing, solvent wash;
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml.Add 50-200mg peroxide or azo-initiator and methyl methacrylate 50-100ml, starting stirring makes initiator be dissolved in monomer, add 2-20g functionalized graphite alkene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 70-90 DEG C, then material is made to maintain about 30 minutes at 70 ~ 85 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 50-60 DEG C, the polymerization of insulation 4-10 low-temperature terminates;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 90-120 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, takes out mould and namely obtains anti-electrostatic synthetic glass.
Graphene described in step one comprises Graphene after Hummer or the standby graphene oxide of modification Hummer legal system or reduction, also can be the graphene oxide with Graphene feature unit structure of other physics or chemical process synthesis, reduced graphene or functionalization graphene;
The quality of the functionalization monomer described in step one and graphene oxide or Graphene and solvent is 1-10:10-30:50-100 than scope;
Catalyzer described in step one is the ester class synthesis reaction catalysts such as hydrochloric acid, sulfuric acid, phosphoric acid, tosic acid;
Initiator described in step 2 is azo or the peroxide catalyzer of radical polymerization, as: Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) and azo-bis-iso-dimethyl, dibenzoyl peroxide, the benzoyl peroxide tert-butyl ester, methylethyl ketone peroxide etc.;
Good solvent described in step one is benzene,toluene,xylene, tetrahydrofuran (THF), phenyl ether, n-butyl ether, dioxane etc.;
Stopper described in step one can be one or more in Resorcinol, Resorcinol, tert-butyl catechol, para benzoquinone, copper naphthenate;
Adopt the teeming practice preparation of segmentation controllable polymerization; Pour in the mould got ready by synthetic glass prepolymer, put in an oven, be warming up to 50-60 DEG C, the polymerization of insulation 4-10 low-temperature terminates, and is slowly warmed up to 90-120 DEG C, is incubated after 1-4 hour and terminates.
The surface resistivity of antistatic organic glass film of the present invention reaches 10
6-10
10q, in antistatic organic glass film of the present invention, antistatic composition is evenly distributed in film simultaneously, and technique is simple, easy to operation, preparation condition is gentle, repetition rate is high, be a kind of permanent type antistatic material, there is stable electrostatic-proof function, remarkable surface hardness and chemical resistance nip performance, transmittance is high, can be used as antistatic material and uses.
Embodiment
embodiment 1: the preparation of graphene oxide
(1) low-temp reaction, adds the vitriol oil of 30mL successively in the beaker of drying, is placed in low-temp reaction bath, treat that the temperature of the vitriol oil is in about 0 DEG C, add graphite 10g under strong mixing, add potassium permanganate 30g several times, control reacting liquid temperature 10 ~ 15 DEG C of stirring reactions two hours;
(2) in, temperature reaction, is placed in 35 DEG C of waters bath with thermostatic control by the beaker of step (1), when question response liquid temp rises to 35 DEG C, continues to stir half an hour;
(3) pyroreaction, under agitation add deionized water, control temperature of reaction within 100 DEG C, continue to stir half an hour, with deionized water by after reaction solution dilution 800 ~ 1000mL, add the hydrogen peroxide of 5%, filtered while hot, hydrochloric acid with 5% and deionized water wash to neutral, after filtration in 50 DEG C of baking ovens dry 48h, obtained graphene oxide.
embodiment 2: the preparation of Graphene
Embodiment 1 gained graphite oxide is mixed with deionized water after grinding is sieved, adding a small amount of ammoniacal liquor is weakly alkaline, sonic oscillation one hour, the ratio adding water is 1mg/1mL, obtains the molten colloidal suspensions of brown color, be the ratio of 10:1 according to the mass ratio of sodium borohydride and graphene oxide, reflux 10h under 100 DEG C of oil baths, obtains black flocks, leaves standstill and filter, dry under room temperature, obtained Graphene.
embodiment 3: the preparation of antistatic organic glass plate
Step one: prepared by functionalized graphite's alkene
Embodiment 1 gained graphene oxide 5.0 grams is dispersed in the 50mL tetrahydrofuran solution of 2.0 grams of vinylformic acid and 50mg Resorcinol, after heating reflux reaction 4h, after underpressure distillation removing tetrahydrofuran (THF), then obtain acrylate functional functionalized graphene after adding 10% aqueous sodium hydroxide solution stirring, filtration, washing.
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml.Add 200mg dibenzoyl peroxide and 100ml methyl methacrylate, starting stirring makes initiator be dissolved in monomer, add 20g acrylic acid functionalized Graphene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 90 DEG C, then material is made to maintain about 30 minutes at 85 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 60 DEG C, be incubated 4 low-temperature polymerizations and terminate;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 120 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, and taking-up mould is taken off sheet glass and namely obtained anti-electrostatic poly (methyl methacrylate) plate.
embodiment 4: Graphene or graphene oxide with the functionalization of glycidyl methacrylate
Step one: prepared by functionalized graphite's alkene
Embodiment 1 gained graphene oxide 5.0 grams is dispersed in the 50mL toluene solution of 2.0 grams of glycidyl methacrylate (GMA) and 50mg Resorcinol, after heating reflux reaction 4h, underpressure distillation removing toluene, then obtain GMA functionalization graphene after adding 10% aqueous sodium hydroxide solution stirring, filtration, washing.
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml.Add 100mg Diisopropyl azodicarboxylate and 100ml methyl methacrylate, starting stirring makes initiator be dissolved in monomer, add 20gGMA functionalized graphite alkene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 90 DEG C, then material is made to maintain about 30 minutes at 85 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 60 DEG C, be incubated 4 low-temperature polymerizations and terminate;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 120 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, and taking-up mould is taken off sheet glass and namely obtained anti-electrostatic poly (methyl methacrylate) plate.
embodiment 5: the preparation of antistatic organic glass plate
Step one: prepared by functionalized graphite's alkene
Embodiment 2 gained Graphene 6.0 grams is dispersed in the 50mL xylene solution of 3.0 grams of vinylformic acid and 50mg Resorcinol, after heating reflux reaction 4h, underpressure distillation except after removal xylene, then obtains acrylate functional functionalized graphene after adding 10% aqueous sodium hydroxide solution stirring, filtration, washing.
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml.Add 100mg Diisopropyl azodicarboxylate and 100ml methyl methacrylate, starting stirring makes initiator be dissolved in monomer, add 20g acrylic acid functionalized Graphene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 85 DEG C, then material is made to maintain about 30 minutes at 70 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 60 DEG C, be incubated 4 low-temperature polymerizations and terminate;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 110 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, and taking-up mould is taken off sheet glass and namely obtained anti-electrostatic poly (methyl methacrylate) plate.
embodiment 6: the preparation of antistatic organic glass plate
Step one: prepared by functionalized graphite's alkene
Embodiment 2 gained Graphene 5.0 grams is dispersed in the 50mL dioxane solution of 1.0 grams of glycidyl methacrylate (GMA) and 50mg Resorcinol, after heating reflux reaction 4h, underpressure distillation removing dioxane, then obtain GMA functionalization graphene after adding 10% aqueous sodium hydroxide solution stirring, filtration, washing.
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml.Add 100mg dibenzoyl peroxide and 100ml methyl methacrylate, starting stirring makes initiator be dissolved in monomer, add 20gGMA functionalized graphite alkene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 90 DEG C, then material is made to maintain about 30 minutes at 85 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 50 DEG C, be incubated 4 low-temperature polymerizations and terminate;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 100 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, and taking-up mould is taken off sheet glass and namely obtained anti-electrostatic poly (methyl methacrylate) plate.
Claims (8)
1. the preparation method of a kind of anti-electrostatic synthetic glass of the present invention carries out according to the following steps:
Step one: prepared by functionalized graphite's alkene
By in graphene oxide or graphene dispersion to the body or its good solvent of acrylic or methacrylic acid glycidyl ester, under the protection of nitrogen and stopper, linked reaction 1-15 hour is carried out under the effect of 30-150 DEG C and catalyzer, remove desolventizing and residual monomer through centrifugation or underpressure distillation, then obtain functionalized graphite's alkene through repeatedly alkali cleaning, washing, solvent wash;
Step 2: prepolymerization
Agitator, prolong, thermometer are installed in the there-necked flask of 250ml;
Add 50-200mg peroxide or azo-initiator and methyl methacrylate 50-100ml, starting stirring makes initiator be dissolved in monomer, add 2-20g functionalized graphite alkene again, dispersed with stirring is even, is incubated 5 minutes when being heated to 70-90 DEG C, then material is made to maintain about 30 minutes at 70 ~ 85 DEG C, observe viscosity, when material be thick, stop stirring by termination reaction below cooling bath abrupt temperature drop to 40 DEG C, prepolymer in there-necked flask is poured in the mould got ready, seals material filling mouth;
Step 3: low temperature polymerization is reacted
Above-mentioned mould is put into baking oven, is warming up to 50-60 DEG C, the polymerization of insulation 4-10 low-temperature terminates;
Step 4: high temperature polymerization is reacted
Mould continues slowly to be warmed up to 90-120 DEG C in an oven, is incubated after 1-4 hour, and baking oven stops heating, gives free rein to be cooled to less than 40 DEG C, takes out mould and namely obtains anti-electrostatic synthetic glass.
2. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, the Graphene that it is characterized in that described in step one comprises Graphene after Hummer or the standby graphene oxide of modification Hummer legal system or reduction, also can be the graphene oxide with Graphene feature unit structure of other physics or chemical process synthesis, reduced graphene or functionalization graphene.
3. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, is characterized in that the quality of the functionalization monomer described in step one and graphene oxide or Graphene and solvent is 1-10:10-30:50-100 than scope.
4. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, is characterized in that the catalyzer described in step one is the ester class synthesis reaction catalysts such as hydrochloric acid, sulfuric acid, phosphoric acid, tosic acid.
5. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, it is characterized in that the initiator described in step 2 is azo or the peroxide catalyzer of radical polymerization, as: Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) and azo-bis-iso-dimethyl, dibenzoyl peroxide, the benzoyl peroxide tert-butyl ester, methylethyl ketone peroxide etc.
6. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, is characterized in that the good solvent described in step one is benzene,toluene,xylene, tetrahydrofuran (THF), phenyl ether, n-butyl ether, dioxane etc.
7. the preparation method of a kind of antistatic organic glass film according to claim 1, is characterized in that the stopper described in step one can be one or more in Resorcinol, Resorcinol, tert-butyl catechol, para benzoquinone, copper naphthenate.
8. the preparation method of a kind of anti-electrostatic synthetic glass according to claim 1, is characterized in that the teeming practice preparation adopting segmentation controllable polymerization; Pour in the mould got ready by synthetic glass prepolymer, put in an oven, be warming up to 50-60 DEG C, the polymerization of insulation 4-10 low-temperature terminates, and is slowly warmed up to 90-120 DEG C, is incubated after 1-4 hour and terminates.
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| CN108410110A (en) * | 2018-05-24 | 2018-08-17 | 安徽新涛光电科技有限公司 | A kind of optical instrument fiber panel functional glass |
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Application publication date: 20160203 |
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| RJ01 | Rejection of invention patent application after publication |