CN109504093A - A kind of preparation method of conductive pressure sensitive nanometer silicon rubber - Google Patents
A kind of preparation method of conductive pressure sensitive nanometer silicon rubber Download PDFInfo
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- CN109504093A CN109504093A CN201811377319.0A CN201811377319A CN109504093A CN 109504093 A CN109504093 A CN 109504093A CN 201811377319 A CN201811377319 A CN 201811377319A CN 109504093 A CN109504093 A CN 109504093A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
- C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of preparation methods of conductive pressure sensitive nanometer silicon rubber, the following steps are included: using deionized water as solution, nontoxic polyvinyl alcohol is added as emulsifier to prepare silicon rubber nano particle, the graphene of electrochemical process preparation is added in the emulsion for containing silicon rubber nano particle later as conductive additive, poly dimethyl oxosilane is added as adhesive, while using the polysorbate 20 of asepsis environment-protecting as the dual conductive emulsifier of emulsifier production.Conductive pressure sensitive nanometer silicon rubber prepared by the present invention can be used as 3D printing or spraying slurry.
Description
Technical field
The present invention relates to new material technology field, in particular to a kind of preparation method of conductive pressure sensitive nanometer silicon rubber.
Background technique
Dimethyl silicone polymer is a kind of macromolecule dimethyl silicone rubber, and there is heat resistance, cold resistance, viscosity to become with temperature
Change small, waterproofness, surface tension it is small, have thermal conductivity, thermal coefficient 0.134-0.159W/M*K, translucency is light transmittance
100%, dimethicone is non-toxic and tasteless, has physiological inertia, good chemical stability.It is electrical insulating property and weatherability, hydrophobic
Property it is good, and have very high anti-shear ability, can be used for a long time at -50 DEG C -200 DEG C.Since it is with good draftability,
Dimethyl silicone polymer silicon rubber is largely used to production Stretch material.However, how to be homogeneously added into conductive filler system
Make conducing composite material and make it have functionality, is still the problem of industry and scientific research circle.
Graphene is a kind of single sheet nano material being made of carbon atom, is made of the carbon atom of sp2 hydridization, and by satisfying
With covalent key connection.Graphene has good electrical and thermal conductivity performance, and resistivity at room temperature is 10-8Ω·m.Preferably because of it
Electric conductivity, light projector, flexibility and mechanical strength.Graphene is in nano-device, microelectronic component, solar battery energy field
With huge application prospect.Then, how high molecular polymer is added in graphene and makes functional material or industry
With the problem of scientific research circle.In particular, how the graphene uniform of addition being dispersed in high molecular polymer and embodying it
Distinctive electric property is highly difficult.The graphene of low concentration is easier to disperse, but they cannot form coherent conduction
System.And the graphene of high concentration is relatively easy to form conductive system, but they will form aggregate in high molecular polymer,
Cause the missing of material function.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of synthetic operation is simple, at low cost and environmentally friendly, efficient production is led
The method of the quick nanometer silicon rubber of voltage.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of preparation method of conductive pressure sensitive nanometer silicon rubber, comprising the following steps:
(1) it selects nontoxic polyvinyl alcohol as emulsifier deionized water as solution, silicon rubber is prepared by emulsion reaction
Glue nano particle emulsion is centrifugated silicon rubber nano particle；
(2) removing oxidation is carried out to graphite material using electrochemical process, prepares graphene platelet；
(3) graphene suspension is added in silicone rubber particles emulsion and makes conductive silicon rubber particle suspension liquid, at this
Polysorbate 20 emulsifier is added in conductive silicon rubber particle emulsion；
(4) liquid poly dimethyl oxosilane is added in the conductive silicon rubber particle emulsion, makes double emulsification
Liquid；
(5) paste is made in the emulsion, the emulsification product of black is put into heater box, passes through chain reaction composite solid state
Conductive pressure sensitive nanometer silicon rubber.
The beneficial effects of the present invention are:
Traditional organic solvent synthetic method is replaced using the emulsion process in aqueous solution, the product that this method obtains mainly contains
Three kinds of ingredients: (1) it is anti-to provide piezoelectricity for silicon rubber nano particle, support needed for providing piezoelectric response, (2) graphene platelet
Required conductive network system is answered, (3) poly dimethyl oxosilane wraps up silicone rubber particles and graphene as adhesive
Come, and provides stronger strongly tensile property to composite material；The preparation method is not only at low cost, environmentally protective but also can efficiently give birth to
It produces, avoids toxic reactant in production process potentially hazardous to environment and human body bring, it can be corresponding to produce according to production requirement
The equipment of energy can be with fast construction, while the property of product, yield can be adjusted flexibly.
Detailed description of the invention
Fig. 1 is the silicon rubber nano particle figure for the emulsion process synthesis that the photo of scanning electron microscope is shown；
Fig. 2 is graphene/poly dimethyl oxosilane silicon rubber nano particulate composite that the photo of scanning electron microscope is shown
Figure；
Fig. 3 is the performance of pressure sensor made of composite material: the relational graph of resistance variations and tensile deformation；
Fig. 4 is the pressing relational graph that pressure sensor made of composite material is used to test finger.
Specific embodiment
The purpose of the present invention is to propose to a kind of preparation methods of conductive pressure sensitive nanometer silicon rubber, comprising the following steps:
Step a: emulsion process silastic elastomer nano particle.7g liquid poly dimethyl oxosilane presoma and 0.7g is taken to solidify
Agent is stirred in the polyvinyl alcohol water solution that mass ratio is 5.83%, which is formed on rotary electronic blender
Pre-emulsion stirs the pre-emulsion with mechanical agitator under the revolving speed of 10000r/min；By the stirring of 40min, formed
After emulsion reaction, which is put into heater box in 50 DEG C of lower heating 8h for milky emulsion, in emulsion
Particles cured poly dimethyl oxosilane silicon rubber nano is solid.
Step b: centrifuge separation silicon rubber nano particle.60g deionized water is added in emulsion, by silicon rubber nano
Grain suspension is put into a centrifuge, and under the revolving speed of 140000r/min, cleaning precipitating, washes away polyvinyl alcohol repeatedly, makes silicon rubber
Glue nanoparticle precipitate object.
Step c: graphene is removed by electrochemical process using the constant voltage reaction kit specially designed.The electrochemical reaction
Instrument uses gravity squash type packed bed, and in the reaction, gravity extruding makes to be capable of forming good contact between graphite particle,
It is good between guarantee electrode to contact and the bubble generated in reaction is smoothly discharged.
In gravity squeezer, design below has opening cavity to promote electrolyte and generate moving freely for gas.
Neutral squeezer design while the reference electrode that can be used for fixing 1M KCl Ag/AgCl, reference electrode pass through gravity squeezer top
Portion is inserted into bottom, and is fixed in this in entire reaction process；The top of reference electrode is on gravity squeezer bottom
At side about 2mm, to the titanium wire circle that diameter is a length of 20cm of 0.25mm is contained in electrode, coil is connected to constant voltage meter, works
Electrode basement is diamond material electrode slice.
Before the reaction working electrode substrate is ultrasonically treated 10min in acetone, washes away surface grease cleaning, then submerge
The 2min in ethyl alcohol, for several times with ultrapure water finally；By working electrode, constant voltage power supply is connected to electrode and reference electrode
On；Then the ammonium sulfate of 80ml and sulfuric acid solution electrolyte are fallen in designed vessel；Pass through nothing in observation confirmation graphite bed
Graphite particle is detached from from graphite bed；The product of the electrochemical stripping is cleaned by centrifugal repeatedly；By
The centrifuge washing of 4400r/min forms the muddy graphite ene product that concentration is 40mg/ml.
Step d: by the graphene mud of above-mentioned preparation, silicon rubber nano particle sediment is mixed.Due to poly- two
Methyl oxosilane liquid cannot be soluble in water, and polysorbate 20 is added in the aqueous mixture as emulsifier, adds liquid
State poly dimethyl oxosilane, forms double emulsion.The mass ratio of each ingredient in the mixture are as follows: silicon rubber nano particle/stone
Black alkene thin slice/polysorbate 20/poly dimethyl oxosilane is 1.5:0.2:0.02:0.6.
Step e: the double emulsion of above-mentioned preparation is stirred evenly using electric mixer.In turning for 10000r/min
20min is persistently stirred under speed, and the paste emulsion product of black is made.Later, which is put into heater box,
2h is heated at 50 DEG C, during which, the poly dimethyl oxosilane of liquid will pass through the poly dimethyl oxosilane of chain reaction composite solid state
Composite material i.e. conductive pressure sensitive nanometer silicon rubber.
Product characteristics explanation:
The apparent of the scanning electron microscope of Fig. 1 shows the diameter of the silicon rubber nano particle of emulsion process synthesis at 0.5-2 μm
Between；
The apparent of the scanning electron microscope of Fig. 1, Fig. 2 shows that there are also equally distributed graphene and silicon rubbers in the composite material
Glue nano particle；
The composite material can be used to make piezoelectric response strain inductor.It is therein when squeezing the composite material
Larger deformation will occur for rubber nano particle, so that the connection status of graphene is driven to change, it is final to generate whole electricity
The variation of resistance.By calculating, it can establish the relationship of pressure deformation and resistance variations as shown in Figure 3, obtain relevant pressure
Sensor.
It can be seen that utilization prospect of the present invention in terms of sensing from the performance of the pressure sensor.By changing composite wood
The size of graphene in material, thus it is possible to vary the sensing sensitivity of the material.The material under highly sensitive can be used for making
Make vital sign sensors.Further, since the product is paste, so it is also used as 3D printing slurry or spraying slurry,
For manufacturing various microelectronics.As shown in figure 4, the material can be used for 3D printing slurry and then make pressure sensitive
Device.
The above content is the further descriptions for combining specific preferred embodiment to be the present invention, are convenient for the skill
The technical staff in art field can understand and apply the invention, and it cannot be said that specific implementation of the invention is only limited to these explanations.It is right
For general technical staff of the technical field of the invention, if can also make without departing from the inventive concept of the premise
Dry simple deduction and replacement, without having to go through creative labor.Therefore, those skilled in the art's announcement according to the present invention,
The simple modifications made to the present invention all should be within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of conductive pressure sensitive nanometer silicon rubber, which comprises the following steps:
(1) select nontoxic polyvinyl alcohol as emulsifier, deionized water prepares silicon rubber by emulsion reaction and receive as solution
Rice grain emulsion is centrifugated silicon rubber nano particle；
(2) removing oxidation is carried out to graphite material using electrochemical process, prepares graphene platelet；
(3) graphene suspension is added in silicone rubber particles emulsion and makes conductive silicon rubber particle suspension liquid, in the conduction
Polysorbate 20 emulsifier is added in silicone rubber particles emulsion；
(4) liquid poly dimethyl oxosilane is added in the conductive silicon rubber particle emulsion, makes double emulsion；
(5) paste is made in the emulsion, the emulsification product of black is put into heater box, passes through leading for chain reaction composite solid state
The quick nanometer silicon rubber of voltage.
2. the preparation method of conductive pressure sensitive nanometer silicon rubber according to claim 1, it is characterised in that:
The emulsion reaction the following steps are included:
(1) taking suitable liquid poly dimethyl oxosilane presoma and curing agent to be stirred in mass percent is 5.83%
In polyvinyl alcohol water solution, the mixed liquor is formed pre-emulsion on rotary electronic blender later；
(2) under the revolving speed of 10000r/min, the pre-emulsion is stirred with mechanical agitator, by the stirring of 40min, forms cream
The emulsion of white；
(3) after emulsion reaction, which is put into heater box heats 8h in 50 DEG C of temperature, poly- in the emulsion
Particles cured dimethyl oxosilane silicon rubber nano is solid.
The centrifuge separation silicon rubber nano particle the following steps are included:
Appropriate amount of deionized water is added in the emulsion.Silicon rubber nano particle suspension liquid is put into a centrifuge,
Under the revolving speed of 140000r/min, by using the cleaning precipitation method repeatedly of low cost, polyvinyl alcohol is washed away, production silicon rubber is received
Rice grain sediment.
3. the preparation method of conductive pressure sensitive nanometer silicon rubber according to claim 1, it is characterised in that:
The use electrochemical process carries out removing oxidation to graphite material, prepare graphene platelet the following steps are included:
(1) removing oxidation is carried out to graphite material using gravity squash type packed bed, in the reaction, gravity extruding makes graphite particle
Between be capable of forming good contact, guarantee good contact between electrode and the bubble generated in reaction be smoothly discharged.
(2) working electrode substrate is ultrasonically treated 10min before the reaction in acetone, surface grease cleaning is washed away, then submerges
The 2min in ethyl alcohol, for several times with ultrapure water finally.By working electrode, constant voltage power supply is connected to electrode and reference electrode
On.Then the ammonium sulfate of 80ml and sulfuric acid solution electrolyte are fallen in designed vessel.By examining confirmation graphite bed
Middle no graphite particle is detached from from graphite bed.The product of the electrochemical stripping can be cleaned by centrifugal repeatedly.
By the centrifuge washing of 4400r/min, the muddy graphite ene product that concentration is 40mg/ml is formed.
4. the preparation method of conductive pressure sensitive nanometer silicon rubber according to claim 1, it is characterised in that:
The production conductive silicon rubber particle suspension liquid the following steps are included:
By the graphene mud of above-mentioned preparation, silicon rubber nano particle sediment is mixed, due to poly dimethyl oxosilane
Liquid cannot be soluble in water, and polysorbate 20 is added in the aqueous mixture as emulsifier, adds liquid poly dimethyl
Oxosilane forms double emulsion.
5. the preparation method of conductive pressure sensitive nanometer silicon rubber according to claim 3, it is characterised in that: the double cream
Change in liquid, reactant ratio are as follows: silicon rubber nano particle/graphene platelet/polysorbate 20/poly dimethyl oxosilane quality
Than for 1.5:0.2:0.02:0.6.
6. the preparation method of conductive pressure sensitive nanometer silicon rubber according to claim 1, it is characterised in that:
The poly dimethyl oxosilane composite material by chain reaction composite solid state the following steps are included:
It by the double emulsion of above-mentioned preparation, is stirred evenly using electric mixer, is persistently stirred under the revolving speed of 10000r/min
20min is mixed, the paste emulsion product of black is made, then the paste emulsion product will be put into heater box, is added at 50 DEG C
Hot 2h, during which, the poly dimethyl oxosilane of liquid will pass through the conductive pressure sensitive nanometer silicon rubber of chain reaction composite solid state.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527221A (en) * | 2019-10-14 | 2019-12-03 | 常州铭仁三维科技有限公司 | A kind of graphene 3D printing material and preparation method thereof |
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| CN1191546A (en) * | 1995-07-25 | 1998-08-26 | 美国3M公司 | Polymerized microemulsion pressure-sensitive adhesive compositions and method of preparing and using same |
| US20050227061A1 (en) * | 2004-04-13 | 2005-10-13 | Research Frontiers Incorporated | Methods for laminating films for SPD light valves and SPD light valves incorporating such laminated films |
| CN102516924A (en) * | 2011-12-07 | 2012-06-27 | 上海应用技术学院 | Conductive organosilicon pressure-sensitive adhesive emulsion and its preparation method |
| CN104151833A (en) * | 2013-10-29 | 2014-11-19 | 泰山医学院 | Preparation method of graphene/silicon rubber pressure-sensitive conductive composite |
| CN108190873A (en) * | 2017-11-23 | 2018-06-22 | 珠海市扬程玻璃制品有限公司 | Prepare the equipment, method and its graphene obtained of graphene |
-
2018
- 2018-11-19 CN CN201811377319.0A patent/CN109504093A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1191546A (en) * | 1995-07-25 | 1998-08-26 | 美国3M公司 | Polymerized microemulsion pressure-sensitive adhesive compositions and method of preparing and using same |
| US20050227061A1 (en) * | 2004-04-13 | 2005-10-13 | Research Frontiers Incorporated | Methods for laminating films for SPD light valves and SPD light valves incorporating such laminated films |
| CN102516924A (en) * | 2011-12-07 | 2012-06-27 | 上海应用技术学院 | Conductive organosilicon pressure-sensitive adhesive emulsion and its preparation method |
| CN104151833A (en) * | 2013-10-29 | 2014-11-19 | 泰山医学院 | Preparation method of graphene/silicon rubber pressure-sensitive conductive composite |
| CN108190873A (en) * | 2017-11-23 | 2018-06-22 | 珠海市扬程玻璃制品有限公司 | Prepare the equipment, method and its graphene obtained of graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527221A (en) * | 2019-10-14 | 2019-12-03 | 常州铭仁三维科技有限公司 | A kind of graphene 3D printing material and preparation method thereof |
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