CN107501455B - Modified static conductive acrylic resin of solvent-free graphene and preparation method thereof - Google Patents
Modified static conductive acrylic resin of solvent-free graphene and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The present invention relates to modified static conductive acrylic resins of a kind of solvent-free graphene and preparation method thereof, this method comprises the following steps: the conductive graphene of the toluene of 20-30g, the methyl methacrylate of 5-10g, the butyl acrylate of 10-20g, the styrene of 25-35g, the acrylic acid of 1-2g, 1-3g being added to heat temperature raising in reactor, temperature is increased to 110-120 DEG C；By catalysts A by being added into reaction kettle, flow back isothermal reaction；In the given time by catalyst B has been added, 110-120 DEG C of isothermal reaction is kept；In the given time by catalyst C has been added, 110-120 DEG C of isothermal reaction is kept；After reaction, it is dehydrated desolventizing, obtains the modified static conductive acrylic materials of required solvent-free graphene.This method by three step polymerization reactions, can efficient uniform ground dispersed graphite alkene, and can preservation stable for a long time, convenient transportation is quick, promotes the extensive use of graphene.
Description
Technical field
The present invention relates to acrylic resins technical fields, and in particular to a kind of modified static conductive third of solvent-free graphene
Olefin(e) acid resin and preparation method thereof.
Background technique
Graphene (Graphene) be one kind by carbon atom with sp2The honeycomb flat film that hybrid form is formed, is one
The quasi- two-dimensional material of only one atomic layer level thickness of kind, does monoatomic layer graphite so being called.Univ Manchester UK's physics
Scholar An Deliegaimu and Constantine's Nuo Woxiao love isolate graphite with micromechanics stripping method success from graphite
Alkene, therefore Nobel Prize in physics in 2010 is obtained jointly.The method of the common power production of graphene is mechanical stripping method, oxygen
Change reduction method, SiC epitaxial growth method, film production method is chemical vapour deposition technique (CVD).Since it is very good strong
Degree, flexible, conductive, thermally conductive, optical characteristics, all in fields such as physics, materialogy, electronic information, computer, aerospaces
Significant progress is arrived.
As presently found most thin, maximum intensity, a kind of strongest novel nano-material of electrical and thermal conductivity performance, graphene
Referred to as " dark fund " is " king of new material ", and scientist even foretells that graphene " will thoroughly change 21 century ".Very likely lift
Play a subversiveness new technology new industrial revolution have swept the globe.
The ultra-high conductivity energy of graphene, can use its this characteristic manufacture conduction, some column coating such as static conductive and
Product.
However, graphene is dispersed into a big difficulty due to the extra specific surface area of graphene, thus limit its
Conductive and static conductive coating industry application.In addition, the Van der Waals force between graphene particle leads to graphene stability
Poor, very easy to reunite, storage is difficult, to affect the effective utilization in later period.
In the Chinese invention patent application application No. is CN201610518036.8, propose a kind of graphene conductive and
The technical solution of static conductive coating application, takes passages as follows: the graphene of 1-5g or so is added to the acrylic acid of 30-40g or so
In resin, the dispersing agent that 1g or so is then added carries out grinding distribution, after graphene dispersion is complete, is added 20-30's or so
Titanium dioxide and other 5-10g fillers, auxiliary agent, 15-20g solvent dispersed, finally obtain product.
However, having following deficiency in the scheme of the patent application:
1, due to the extra specific surface area of graphene, dispersion of the graphene in acrylic resin at this stage is still had any problem,
And need to be dispersed with stirring for a long time, the time is long, low efficiency；
2, graphene acrylic resin syrup saves difficult, and reunion and deposited phenomenon occur quickly, influences the use in later period；
3, solvent type graphene acrylic resin syrup belongs to harmful influence, transport, and storage is inconvenient.
Summary of the invention
In view of this, providing a kind of high efficiency dispersion graphene, stable for a long time capable of saving, convenient transportation efficiently solvent-free stone
Modified static conductive acrylic resin of black alkene and preparation method thereof.
A kind of modified static conductive acrylic resin preparation method of solvent-free graphene, it includes following mass percentages
Component:
By the benzene second of the toluene of 20-30g, the methyl methacrylate of 5-10g, the butyl acrylate of 10-20g, 25-35g
Alkene, the acrylic acid of 1-2g, 1-3g conductive graphene be added to heat temperature raising in reactor, temperature is increased to 110-120 DEG C；
A reaction: at 110-120 DEG C, by the way of by adding, reaction is added in reaction 1-2g catalyst A in 2-3h
In kettle, flow back isothermal reaction 1.5-2h, and in A reaction, polymer molecular weight control is within the scope of 50000-60000；
B reaction: after the A reaction time reaches, in the given time by 0.5-1g catalyst B has been added, 110-120 is kept
DEG C isothermal reaction 1.5-2h, in B reaction, polymer molecular weight control is within the scope of 70000-80000；
C reaction: after the B reaction time reaches, in the given time by 0.1-0.5g catalyst C has been added, 110- is kept
120 DEG C of isothermal reaction 0.5-1h, in C reaction, polymer molecular weight control is within the scope of 7500-9000；
C after reaction, be dehydrated desolventizing, obtain the modified static conductive acrylic resin material of required solvent-free graphene
Material.
And a kind of modified static conductive acrylic resin of solvent-free graphene, use solvent-free graphite as described above
The modified static conductive acrylic resin preparation method of alkene is made.
In the above-mentioned modified static conductive acrylic resin preparation method of solvent-free graphene, by conductive graphene and polymerized monomer
It mixes together in the reactor, in polymerization process, graphene can be in conjunction with intermediate condensate, such as passes through hydroxyl or carboxylic
Base junction closes graphene, to play the role of dispersed graphite alkene.Further, by the way that polymerization reaction is divided into three steps, respectively
Using different catalyst, in every step reaction process, graphene all can be in conjunction with condensate.Due to three steppings of polymerization reaction point
Row, all rightly control is unlikely to allow the molecule of polymer to allowing the molecular weight of polymer to reach predetermined amount to the reaction of every step
Successively increase, the polymerization reaction of second step and third step reaction mainly residual monomer, in this way, making the molecule of polymer
Distribution uniform is measured, distribution is relatively narrow, and the molecular weight distribution of polymer is wider when avoiding one-step polymerization in the prior art, and
The excessively high deficiency of partial polymer molecular weight.In this way, the polymer molecule size that the above method is formed controls relatively narrow range, and
And graphene is all in conjunction with the polymer in the step in every step, since polymer molecule size is more uniform, so that stone
The dispersion of black alkene is also more uniform, thus the efficient uniform ground dispersed graphite alkene in acrylic resin, and can guarantee prolonged
Storage stability, after saving 1 year, sheet resistance value is basically unchanged, in client's transport, convenient to use, save the cost.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of modified static conductive acrylic resin preparation method of solvent-free graphene comprising such as
Lower step:
By the benzene second of the toluene of 20-30g, the methyl methacrylate of 5-10g, the butyl acrylate of 10-20g, 25-35g
Alkene, the acrylic acid of 1-2g, 1-3g conductive graphene be added to heat temperature raising in reactor, temperature is increased to 110-120 DEG C；
A reaction: at 110-120 DEG C, by the way of by adding, catalysts A being added in reaction kettle in 2-3h,
Flow back isothermal reaction 1.5-2h；
B reaction: after the A reaction time reaches, in the given time by catalyst B has been added, 110-120 DEG C of constant temperature is kept
React 1.5-2h；
C reaction: after the B reaction time reaches, in the given time by catalyst C has been added, 110-120 DEG C of constant temperature is kept
React 0.5-1h；
C after reaction, be dehydrated desolventizing, obtain the modified static conductive acrylic resin material of required solvent-free graphene
Material.
Wherein, it when the first step mixes, stirs by mixing simultaneously, is heated to 110-120 DEG C while stirring.
In A reaction, the catalysts A is peroxidized t-butyl perbenzoate, and the time is added dropwise in dosage 1-2g
Catalyst A is added, since addition that is, after temperature reaches 110-120 DEG C in preferably 2.5-3 hours, more preferably 3 hours
It is 3h to addition end time span.In this reaction process, the main initiated polymerization of catalyst A, polymer point when this is reacted
Son amount range is about 50000-60000, and it is to be further continued for after dripping catalyst instead that the time of the A reaction, which is preferably 2h,
Answer 2h.
In B reaction, the catalysts B is peroxidized t-butyl perbenzoate, and it is excellent to add the time by dosage 0.5-1g
It is selected as 10-30min, more preferably 15min.The time of B reaction is 2h, and in this reaction process, catalyst B, which further causes, to be gathered
Reaction is closed, polymer molecular weight range is about 70000-80000 when this is reacted.
In C reaction, the catalysts C is peroxidized t-butyl perbenzoate, and dosage 0.1-0.5g adds the time
Preferably 10-30min, more preferably 15min, i.e., since addition to addition end time span be 15min.The C reaction
Time is preferably 1h, i.e., after addition finishes catalyst, is maintained at 110-120 DEG C of isothermal reaction 1h.In this reaction process, catalysis
Agent C continues initiated polymerization, and polymer molecular weight range is about 75000-90000 when this is reacted.Above-mentioned A reaction, B are anti-
It answers, in C reaction, on the one hand catalyst A, catalyst B and catalyst C, which are both preferably peroxidized t-butyl perbenzoate, to be made for one
Reaction controlling more secure and reliable, on the other hand, so that reaction product is also relatively stable, it is easier to control.
Preferably, it in each reaction process that A reaction, B reaction, C react, is measured after predetermined reaction time respectively poly-
Adduct molecule amount controls reaction process according to the polymer molecular weight of measurement.The embodiment of the present invention is not only by stepwise reaction
Control polymerization reaction, regulate and control the molecular weight of polymer, moreover, by the dosage for controlling each step catalyst, and using by
Step reasonably reduces the dosage of catalysts, and controlledly to reduce polymerization rate, control molecular weight increases.Specifically
Ground, the time of measurement can be at interval of 10-30 minutes, once measurement result show polymer molecular weight have it is higher in predetermined value
When, that is, stop reaction or pause reaction.
In the above-mentioned modified static conductive acrylic resin preparation method of solvent-free graphene, by conductive graphene and polymerized monomer
It mixes in the reactor, in polymerization process, A reaction, B is reacted, in C reaction, by the given time together
Catalyst is added dropwise, so that reaction is all more leniently to carry out, avoids adding multi-catalyst and reaction being caused acutely to cause
Polymerization is uneven, moreover, reaction can all generate water, facilitates the evaporation of water at 110-120 DEG C, promotes reaction is lasting to carry out.
Specifically, in first step reaction, polymerization reaction between polymerized monomer passes through the control and catalysis in reaction time
The control of agent, the polymer molecular weight narrow distribution of formation, and molecular weight is smaller, exists by measuring basic control molecular weight distribution
50000-60000 range is effectively prevented from bigger molecule or super high molecular weight polymer in the first step and generates.
In second step reaction, according to Principles of Polymerization, the remaining unreacted polymerized monomer of the first step is first reacted,
The polymer that the first step generates will less participate in reacting, and the speed that second step enters catalyst dropwise is very fast with respect to the first step, and
And by the control reaction time, remaining polymerized monomer reaction is substantially set to carry out polymerization reaction, while monitoring molecular weight, substantially
In 70000-80000 range, when reaching above range, that is, stop reaction.
In third step reaction process, the speed for entering catalyst dropwise is very fast with respect to the first step, reacts basic with second step
It is similar, since after two-step reaction, polymerized monomer residue is smaller, so the dosage of catalyst is controlled in 0.1-0.5g, still
The addition time is essentially identical with second step, and the reaction time is also relatively short, and similarly, according to Principles of Polymerization, second step is surplus
Remaining unreacted polymerized monomer is first reacted, and the polymer that first two steps generate will less participate in reacting, while monitor molecule
Amount when reaching above range, that is, stops reaction substantially in 75000-90000 range.
In the reaction of every step, graphene can in conjunction with intermediate condensate, such as by hydroxy or carboxy combination graphene, from
And play the role of dispersed graphite alkene.Since polymerization reaction is carried out in three steps, every step reaction all rightly controls poly- to allowing
The molecular weight for closing object reaches predetermined amount, and the molecular weight distribution of polymer is relatively narrow.In this way, the polymer molecule that the above method is formed is big
The relatively narrow range of small control, moreover, graphene is all in conjunction with the polymer in the step in every step, due to polymer molecule size
More uniformly, carrier of the polymer molecule as graphene, distribution is more uniform, and the dispersion of graphene is also more uniform, thus
Efficient uniform ground dispersed graphite alkene in acrylic resin, and can guarantee prolonged storage stability, in client's transport, user
Just quick, save the cost.
Above-mentioned vacuum dehydration, desolventizing pours out material up to water and solvent removal under high temperature after reaction, cooling
After crush, film-making or be granulated after packed preservation.
The embodiment of the present invention also provides a kind of modified static conductive acrylic resin of solvent-free graphene, uses as described above
The modified static conductive acrylic resin preparation method of solvent-free graphene be made.The modified static conductive third of the solvent-free graphene
Olefin(e) acid resin is graininess.In use, directly by the modified static conductive acrylic acid of the solvent-free graphene prepared according to the above method
Stirring and dissolving after resin particle and filler, auxiliary agent, solvent mixing, can be obtained corresponding coating products or solvent-free products.
By measurement, the resistivity substantially 8*10 of the modified static conductive acrylic resin of solvent-free graphene3Ω·m-2*
105Ω·m。
Embodiment one
The modified static conductive acrylic resin preparation method of the solvent-free graphene of embodiment 1, includes the following steps:
One stage: by the toluene of 20g, the methyl methacrylate of 5g, the butyl acrylate of 10g, the styrene of 25g, 1g
Acrylic acid, 1g conductive graphene be added to heat temperature raising in reaction kettle, temperature is increased to 110-120 DEG C.
Two-stage: after temperature reaches 110-120 DEG C of setting value, by the way of by adding, by the anti-of 1g in 3h or so
Catalyst A is answered to be added in reaction kettle, flow back isothermal reaction 2h.
Three stages: after the reaction time reaches, 0.5g catalyst B, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 2h.
Four stages: after the reaction time reaches, 0.1g catalyst C, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 1h.
After reaction, vacuum dehydration, desolventizing, up to pouring out material, powder after cooling under water and solvent removal, high temperature
It is broken, packed preservation after film-making or granulation.
In use, corresponding coating products directly can be obtained in stirring and dissolving after this product and filler, auxiliary agent, solvent mixing
Or solvent-free products.
Test: the modified static conductive acrylic resin initial surface resistivity value of test solvent-free graphene obtained is 5*105
Ω m, then by after the solvent-free graphene modified the preservation of static conductive acrylic resin 1 year, initial surface electricity is tested in dissolution spraying
Resistance value is 7.8*105Ω m, it is undifferentiated compared with the resin surface resistance before preservation.
Embodiment two
The embodiment of the present invention provides a kind of modified static conductive acrylic resin preparation method of solvent-free graphene comprising such as
Lower step:
One stage: by the toluene of 25g, the methyl methacrylate of 6g, the butyl acrylate of 12g, the styrene of 28g, 1g
Acrylic acid, 1g conductive graphene be added to heat temperature raising in reaction kettle, temperature is increased to 110-120 DEG C.
Two-stage: after temperature reaches 110-120 DEG C of setting value, by the way of by adding, by 1.2g's in 3h or so
Catalysts A is added in reaction kettle, and flow back isothermal reaction 2h.
Three stages: after the reaction time reaches, 0.6g catalyst B, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 2h.
Four stages: after the reaction time reaches, 0.2g catalyst C, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 1h.
After reaction, vacuum dehydration, desolventizing, up to pouring out material, powder after cooling under water and solvent removal, high temperature
It is broken, packed preservation after film-making or granulation.
In use, corresponding coating products directly can be obtained in stirring and dissolving after this product and filler, auxiliary agent, solvent mixing
Or solvent-free products.
Test: the modified static conductive acrylic resin initial surface resistivity value of test solvent-free graphene obtained is 3*105
Ω m, then by after the solvent-free graphene modified the preservation of static conductive acrylic resin 1 year, initial surface electricity is tested in dissolution spraying
Resistance value is 4.5*105Ω m, it is undifferentiated compared with the resin surface resistance before preservation.
Embodiment three
The embodiment of the present invention provides a kind of modified static conductive acrylic resin preparation method of solvent-free graphene comprising such as
Lower step:
One stage: by the toluene of 28g, the methyl methacrylate of 7g, the butyl acrylate of 15g, 30g styrene,
The acrylic acid of 1.5g, the conductive graphene of 1.5g are added to heat temperature raising in reaction kettle, and temperature is increased to 110-120 DEG C.
Two-stage: after temperature reaches 110-120 DEG C of setting value, by the way of by adding, by 1.5g's in 3h or so
Catalysts A is added in reaction kettle, and flow back isothermal reaction 2h.
Three stages: after the reaction time reaches, 0.8g catalyst B, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 2h.
Four stages: after the reaction time reaches, 0.3g catalyst C, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 1h.
After reaction, vacuum dehydration, desolventizing, up to pouring out material, powder after cooling under water and solvent removal, high temperature
It is broken, packed preservation after film-making or granulation.
In use, corresponding coating products directly can be obtained in stirring and dissolving after this product and filler, auxiliary agent, solvent mixing
Or solvent-free products.
Test: the modified static conductive acrylic resin initial surface resistivity value of test solvent-free graphene obtained is 7*104
Ω m, then by after the solvent-free graphene modified the preservation of static conductive acrylic resin 1 year, initial surface electricity is tested in dissolution spraying
Resistance value is 9.2*105Ω m, it is undifferentiated compared with the resin surface resistance before preservation.
Example IV
The embodiment of the present invention provides a kind of modified static conductive acrylic resin preparation method of solvent-free graphene comprising such as
Lower step:
One stage: by the toluene of 30g, the methyl methacrylate of 8g, the butyl acrylate of 20g, the styrene of 35g, 2g
Acrylic acid, 2g conductive graphene be added to heat temperature raising in reaction kettle, temperature is increased to 110-120 DEG C.
Two-stage: after temperature reaches 110-120 DEG C of setting value, by the way of by adding, by the anti-of 2g in 3h or so
Catalyst A is answered to be added in reaction kettle, flow back isothermal reaction 2h.
Three stages: after the reaction time reaches, 1g catalyst B, 15min or so is added by having added, then at 110-120 DEG C
Isothermal reaction 2h.
Four stages: after the reaction time reaches, 0.5g catalyst C, 15min or so is added by having added, then in 110-120
DEG C isothermal reaction 1h.
After reaction, vacuum dehydration, desolventizing, up to pouring out material, powder after cooling under water and solvent removal, high temperature
It is broken, packed preservation after film-making or granulation.
Test: the modified static conductive acrylic resin initial surface resistivity value of test solvent-free graphene obtained is 6*105
Ω m, then by after the solvent-free graphene modified the preservation of static conductive acrylic resin 1 year, initial surface electricity is tested in dissolution spraying
Resistance value is 8.1*105Ω m, it is undifferentiated compared with the resin surface resistance before preservation.
It should be noted that the invention is not limited to above embodiment, creative spirit according to the present invention, this field
Technical staff can also make other variations, and the variation that these creative spirit according to the present invention are done should all be included in this hair
It is bright it is claimed within the scope of.
Claims (9)
1. a kind of modified static conductive acrylic resin preparation method of solvent-free graphene, which is characterized in that it includes the following steps:
By the toluene of 20-30g, the methyl methacrylate of 5-10g, the butyl acrylate of 10-20g, the styrene of 25-35g, 1-
The acrylic acid of 2g, the conductive graphene of 1-3g are added to heat temperature raising in reactor, and temperature is increased to 110-120 DEG C；
A reaction: at 110-120 DEG C, by the way of by adding, 1-2g catalysts A being added in reaction kettle in 2-3h,
Flow back isothermal reaction 1.5-2h, and in A reaction, polymer molecular weight control is within the scope of 50000-60000；
B reaction: after the A reaction time reaches, in the given time by 0.5-1g catalyst B has been added, 110-120 DEG C of perseverance is kept
Temperature reaction 1.5-2h, in B reaction, polymer molecular weight control is within the scope of 70000-80000；
C reaction: after the B reaction time reaches, in the given time by 0.1-0.5g catalyst C has been added, kept for 110-120 DEG C
Isothermal reaction 0.5-1h, in C reaction, polymer molecular weight control is within the scope of 7500-9000；
C after reaction, be dehydrated desolventizing, obtain the modified static conductive acrylic materials of required solvent-free graphene.
2. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that institute
Stating catalysts A is peroxidized t-butyl perbenzoate, is 2.5-3 hours by the predetermined time is added.
3. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that institute
Stating catalysts B is peroxidized t-butyl perbenzoate, is 10-30min by the predetermined time is added.
4. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that institute
Stating catalysts C is peroxidized t-butyl perbenzoate, is 10-30min by the predetermined time is added.
5. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that institute
The time for stating A reaction is 1.8-2h, and the time of the B reaction is 1.8-2h, and the time of the C reaction is 0.8-1h.
6. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that
It is cooling after being dehydrated desolventizing, it crushes, film-making or granulation.
7. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that
In each reaction process that A reaction, B reaction, C react, polymer molecular weight is measured after predetermined reaction time respectively, according to survey
Fixed polymer molecular weight controls each reaction process.
8. the modified static conductive acrylic resin preparation method of solvent-free graphene as described in claim 1, which is characterized in that system
The resistivity of the modified static conductive acrylic materials of the solvent-free graphene obtained is 2.5*105Ω·m-6*103Ω·m。
9. a kind of modified static conductive acrylic resin of solvent-free graphene, which is characterized in that the solvent-free graphene modification is led
Electrostatic acrylic resin is using the modified static conductive acrylic resin of solvent-free graphene as described in claim 1-8 any one
Preparation method is made.
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| CN106915740A (en) * | 2017-05-08 | 2017-07-04 | 同光（江苏）新材料科技有限公司 | A kind of preparation method of graphene dispersing solution |
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Effective date of registration: 20181220 Address after: Yangkou Port Lingang Industrial Zone, Changsha Town, Rudong County, Jiangsu Province Patentee after: Jiangsu Doupeng Technology Co., Ltd. Address before: 226000 Shop 104, North Building, Xinguang Community Center, 333 Changjiang Road, Diggang Town, Rudong County, Nantong City, Jiangsu Province Patentee before: Jiangsu Rudong high-tech graphite Industry Research Institute Co., Ltd. |
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Inventor after: Pan Zuo Inventor after: Zhou Haiyan Inventor after: Wang Dongdong Inventor before: Zhou Haiyan Inventor before: Wang Dongdong |