CN104530833B - A kind of organosilicon electrically conductive ink - Google Patents
A kind of organosilicon electrically conductive ink Download PDFInfo
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- CN104530833B CN104530833B CN201410806529.2A CN201410806529A CN104530833B CN 104530833 B CN104530833 B CN 104530833B CN 201410806529 A CN201410806529 A CN 201410806529A CN 104530833 B CN104530833 B CN 104530833B
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- silicone oil
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Silicon Polymers (AREA)
Abstract
The invention belongs to macromolecule and electrically conductive ink technical field, relate to a kind of organosilicon electrically conductive ink.Electrically conductive ink is formed by polymerizable organosilicon monomer, conductive material and catalyst are jointly compounding.Wherein polymerizable organosilicon monomer is collectively constituted by end-vinyl block silicone oil II and containing hydrogen silicone oil I, and conductive material is collectively constituted by conductive black and graphite powder, and catalyst is chloroplatinic acid.In formula: a=5～20, b=5～20, m=100～500；X=1～10；Y=5～30.
Description
Technical field
The invention belongs to macromolecule and electrically conductive ink technical field, be specifically related to a kind of organosilicon electrically conductive ink.
Background technology
Electrically conductive ink good conductivity, low cost, advantages of nontoxic raw materials or low toxicity are high with base material binding strength, easy to use, and by
Step Substitute For Partial metallic circuit, in photovoltaic industry, printed circuit, biosensor, electromagnetic shielding material, ID card, RFID antenna
Extensively apply in field.Electrically conductive ink starts to use, for printing electrically conductive circuits at emerging fields such as intelligent textiles in recent years
With the purposes such as antistatic coating, but this conducting channel and antistatic coating not wash resistant, non-fold resistant, service life is short,
Impact popularizes.In order to overcome disadvantages mentioned above, need conducting ink formulation is improved, with improve its on the textile should
Washable, the folding quality of used time, increases the service life.
Presently commercially available electrically conductive ink kind is a lot, and the most common Acheson423SS, CH-8 etc. have the conduction of excellence
Performance, in PET film, printed coating can bend 180-360 °, but can not be folding.These electrically conductive inks are printed
On the textile, conductive coating not wash resistant, the most not fold resistant.
Iida Kazani etc., at Fibres&Textiles in Eastern Europe, carry in 2012,20 (1): 57-63
Arrive, smear one layer of silver-colored electrically conductive ink at textile surface, measure coating washing fastness, after washing 20 times in washing machine, part
The conductive coating of sample comes off, and the resistance value of remaining sample increases 60-1500 times, and all samples is the most washable.If in conduction
One layer of protective polyurethane layer of the surface-coated of coating, then sample washing fastness increases, and after washing 20 times, has in washing machine
The resistance value of two samples only improves 10-25%, it is believed that washable 20 times, but this also has the biggest with the standard of washable 50 times
Gap.
Up to the present, there is not yet can use on the textile, can washable 50 times, be resistant to 180 ° of folding conductions
The document report of ink.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that the organosilicon conductive oil of a kind of wash resistant fold resistant
Ink.
The technical solution used in the present invention is for achieving the above object:
A kind of organosilicon electrically conductive ink of wash resistant fold resistant, by weight percentage, electrically conductive ink having by 60-85%
Machine silicon polymerization monomer, 10-35% conductive material and 0.01-5% catalyst are jointly compounding to be formed；
Wherein, polymerizable organosilicon monomer is collectively constituted by end-vinyl block silicone oil II and containing hydrogen silicone oil I；Conductive material by
Conductive black and graphite powder collectively constitute；Catalyst is the aqueous isopropanol of chloroplatinic acid；
In formula:
A=5-20, b=5-20, m=100-500；X=1-10；Y=5-30.
Organosilicon electrically conductive ink preferred, by weight percentage, electrically conductive ink is by the polymerizable organosilicon list of 65-80%
Body, 19-34% conductive material and 0.1-1% catalyst are jointly compounding to be formed.
The preparation reaction of described end-vinyl block silicone oil II is as follows:
In formula: a=5-20, b=5-20, m=100-500；
Hydrogeneous phenyl silicone oil IV is reacted 2-20 hour at 80-150 DEG C with vinyl-terminated silicone fluid III in the presence of a catalyst, raw
Become end-vinyl block silicone oil II；
Wherein, hydrogeneous phenyl silicone oil IV is 1:2-3 with the mol ratio of vinyl-terminated silicone fluid III；The addition of catalyst is for leading
The 0.01-5% of electricity ink by weight；Catalyst is the aqueous isopropanol of chloroplatinic acid.
The preparation of end-vinyl block silicone oil II preferably, hydrogeneous phenyl silicone oil IV in the presence of a catalyst with end ethylene
Base silicone oil III reacts 3-12 hour at 100-130 DEG C, generates end-vinyl block silicone oil II；
Wherein, hydrogeneous phenyl silicone oil IV is 1:2 with the mol ratio of vinyl-terminated silicone fluid III；The addition of catalyst is conduction
The 0.1-1% of ink by weight.
In described end-vinyl block silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of reactive hydrogen is 1:1-20.Contain
Hydrogen silicone oil I can be partly by commercially available acquisition, it is also possible to prepare according to method well known in the art.
Preferably, in end-vinyl block silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of reactive hydrogen is 1:1-5.
In described conductive material, the weight ratio of conductive black and graphite powder is 1:1-10.Conductive black and graphite powder can lead to
Cross commercially available acquisition.
Preferably, in described conductive material, the weight ratio of conductive black and graphite powder is 1:1-7.
Described graphite powder is the high-purity graphite powder of purity >=99.85%, its particle mean size≤30 μm.
A kind of application of the organosilicon electrically conductive ink of wash resistant fold resistant, the organosilicon conductive oil of described wash resistant fold resistant
Ink is applied in textile antistatic or conducting channel.
Advantage for present invention: be printed on the base materials such as textile by the organosilicon electrically conductive ink of the present invention, through solid
After changing crosslinking, forming netted silicone resin coating, good with the base material binding strength such as textile, feel is the most soft, it is possible to warp
By folding and do not damage, washing resistance performance is far better than the electrically conductive ink using polyacrylic resin.
The organosilicon electrically conductive ink of wash resistant fold resistant of the present invention is used for textile antistatic or conducting channel etc.
Purposes.Owing to its electric conductivity is relatively good, during conductive coating thickness 30 microns, sheet resistance is in 103-104Ω/sq scope, is spinning
Print on fabric and after the crosslinking that is heating and curing, coating uniform, soft, flexible.If using the graphite powder that granule is less,
Just can be made to thinner by printed coating thickness in application process, this is to product marketing advantageously.
Electrically conductive ink of the present invention, when printing on the textile, the end-vinyl block silicone oil II in ink and containing hydrogen silicone oil I
Heated solidification is cross-linked to form space network, the washable silicone resin coating of resistance to fold-type obtained.Coating is combined with fiber
Fastness is high, has the distinctive flexibility of organosilicon；And the phenyl silica block in molecule can effectively promote coating hardness, compose
Scratch-resistant, the anti-wear performance that precoat is special, can bear the friction repeatedly of inner tank of washing machine, and dryer when drying when washing
The friction repeatedly of inner core and shock, it is ensured that coating is repeatedly washed and do not damaged.The electrically conductive ink of the present invention is applied on the textile
Time, conductive coating can wash with washing machine, can be folding, and coating is long for service life.Specifically:
1, wash resistant: on the textile after printing, is amenable to 50 washings of washing machine and conductive coating stands intact, washing
The change of rear coated conductive is less than ± 20%.
2, fold resistant: on the textile after printing, be amenable to 180 ° folding, and conductive coating occurs without slight crack, folding
After folded 3000 times, coated conductive change is less than ± 20%.
3, electric conductivity: using the conductive material such as white carbon black and graphite powder, sheet resistance is up to 103-105(conduction is coated with Ω/sq
Layer thickness 30 μm).
4, impressionability energy: available conventional screen printing mode is in textile surface printing, very easy to use.
Accompanying drawing explanation
The conducting sample that Fig. 1 a-h provides for the embodiment of the present invention.
Fig. 2 washs the design sketch before and after 50 times for the conducting sample that the embodiment of the present invention provides, and wherein a is for using the present invention
After before conductive coating washing, sample, b wash 50 times for employing conductive coating of the present invention, sample, c are for using comparative example conductive coating
Wash the sample after 50 times.
The conducting sample that Fig. 3 provides for the embodiment of the present invention fold before and after design sketch, wherein a is for using present invention conduction
Coating folds front sample, b is employing conductive coating folded swatch of the present invention, c is the sample after using comparative example conductive coating to fold
Product.
Detailed description of the invention
In order to be better understood from the present invention, below in conjunction with embodiment, the invention will be further elaborated, but the present invention
It is only limitted to absolutely not this.
Polymerizable organosilicon monomer of the present invention is collectively constituted by end-vinyl block silicone oil II and containing hydrogen silicone oil I, if in order to
Reduce cost, replace end-vinyl block silicone oil II by end-vinyl phenyl silicone oil common on market, then washing fastness is obvious
Declining, do not reach the requirement of washable 50 times, folding quality also declines.Equally, in order to reduce cost purpose, with the end without phenyl
Vinyl methyl silicone oil replaces end-vinyl block silicone oil II, then coating washing fastness is the most very poor, and coating is after cyclic washing
It is damaged, does not reaches the requirement of washable 50 times.
Conductive material of the present invention is collectively constituted by conductive black and graphite powder, in order to improve the conduction of organosilicon electrically conductive ink
Performance, the weight ratio of the two is 1:1-10, preferably 1:1-7；Ratio is too high or too low, and electric conductivity is all decreased obviously.If individually
Use conductive black or graphite powder, then electric conductivity is worse.In order to promote electric conductivity, graphite powder used be purity >=
The high-purity graphite powder of 99.85%, the graphite powder poorly conductive that purity is low, should not use.Particle mean size≤30 μm of graphite powder,
So just it is not easy network blocking when using the mode printing conductive inks such as silk screen printing.Conductive black includes commercially available
Various model conductive blacks, pay the utmost attention to the conductive black that good conductivity, granularity are thin, the common trade mark include BP2000,
VXC-72R, VXC-72, AS-300J, EC-600JD, EC-300J, 3350B, T-90 etc..
Catalyst is chloroplatinic acid, can be configured to platinum acid chloride solution in advance for convenience of using, and conventional is chloroplatinic acid isopropyl
Alcoholic solution, concentration is 0.01-5% (w/w), preferably 0.1-1%.Want appropriate when using catalyst, add the catalyst meeting of excess
Shortening the period of storage of electrically conductive ink, the electrically conductive ink shelf-life of the present invention is room temperature about 1 year, leads after adding excess catalyst
Within the period of storage of electricity ink can shorten to 6 months.High activity amines catalyst should not use, otherwise the storage of electrically conductive ink
Time can be the shortest, affects its commercial value.
The organosilicon electrically conductive ink of described wash resistant fold resistant is applied in textile antistatic or conducting channel.The present invention
Organosilicon electrically conductive ink is different from commercially available electrically conductive ink, and commercially available electrically conductive ink is usually added into a certain amount of solvent, for molten
Solve resin and increase mobility, and conductive material being uniformly dispersed, as in Acheson423SS, CH-8, solvent accounts for the one of gross weight
Half left and right, but the organosilicon electrically conductive ink of the present invention does not allows to add too much solvent.Such as quantity of solvent reaches 5%, will
Having influence on the solidification cross-linking effect of organic silicon monomer, coating is washable and folding quality all significantly reduces.
Raw material used in the embodiment of the present invention is commercially available, it is also possible to according to side well known to the skilled artisan in the art
Formula prepares.C in formula6H5-represent phenyl.
The washing fastness of the organosilicon electrically conductive ink of the present invention is used standard method test (BS EN ISO6330:
2012)。
Fold resistant performance uses the test of the domestic HT-1063 machine of resistance to bending and unbending test.
Experimental drug:
Vinyl-terminated silicone fluid ... ... ... industrial goods, 99%
Hydrogeneous phenyl silicone oil ... ... ... make by oneself in the following manner, 99%
Containing hydrogen silicone oil ... ... ... .... industrial goods, 99%
End-vinyl phenyl silicone oil ... ... ... ... industrial goods, 99%
Conductive black ... ... ... ... ... ... industrial goods
Graphite powder ... ... ... ... ... ... purity >=99.85%, particle mean size≤30 μm
2-Butoxyethyl acetate ... ... ... industrial goods, 99%
Chloroplatinic acid ... ... ... ... industrial goods, 99%
Isopropanol ... ... ... ... .. analytical pure, 99%
0.2% chloroplatinic acid catalyst (2 grams of chloroplatinic acids are dissolved in 998 grams of isopropanols, are made into 0.2% solution)
The reference preparation method of hydrogeneous phenyl silicone oil:
Equipped with agitator, thermometer, reflux condensing tube four mouthfuls of round-bottomed flasks in, add requirement tetramethyl dihydro
Disiloxane and octamethylcy-clotetrasiloxane, be warming up to desired reaction temperature (such as 50-80 DEG C), add a small amount of dense sulfur under stirring
Acid, insulation reaction 2-4 hour, it is subsequently adding the octaphenylcyclotetrasiloxane of requirement, then reacts 2-8 hour.It is cooled to room temperature,
Neutralize with natrium carbonicum calcinatum, solids removed by filtration thing.Filtrate in 120-150 DEG C with water pump-0.095MPa vacuum removal low-boiling-point substance,
I.e. obtain hydrogeneous phenyl silicone oil.
Preparation embodiment
Embodiment 1
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 73.04% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.74% |
| 3 | Conductive black | 11.5 | 5% |
| 4 | Graphite powder | 46 | 20% |
| 5 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.22% |
| Add up to 100% |
Organosilicon electrically conductive ink can form a kind of netted washable folding resistance organosilicon tree in the cross-linking process that is heating and curing
Fat, reaction equation is as follows:
The concrete preparation process of organosilicon electrically conductive ink is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=100, molecular weight about 7602) as shown in formula III is added to reaction
Bottle, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stirs.It is warming up to 120 DEG C, slowly drips
Add 0.01 mole of structure hydrogeneous phenyl silicone oil (a=5, b=5, molecular weight about 1496.6) as shown in formula IV, within 2 hours, add, then protect
Temperature reaction 4 hours, completes reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl block as shown in formula II
Silicone oil, weighs 168 grams, wherein a=5, b=5, m=100；Molecular weight about 16,701.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into 11.5 grams to lead
Electricity white carbon black and 46 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtaining 230 grams of black paste has
Machine silicon electrically conductive ink.Wherein a=5, b=5, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 8000-10000mPa.s/25 DEG C.
Embodiment 2
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 67.2% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.6% |
| 3 | Conductive black | 10 | 4% |
| 4 | Graphite powder | 67.5 | 27% |
| 5 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.2% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method: same as in Example 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, 10 it are slowly added into
Gram conductive black and 67.5 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain 250 grams of black
Pasty state organosilicon electrically conductive ink.Wherein a=5, b=5, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 5000-7000mPa.s/25 DEG C.
Embodiment 3
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 74.78% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.78% |
| 3 | Conductive black | 17.97 | 8% |
| 4 | Graphite powder | 33.7 | 15% |
| 5 | 0.2% chloroplatinic acid catalyst | 1 | 0.44% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method: same as in Example 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, 17.97 it are slowly added into
Gram conductive black and 33.7 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain 224.67 grams black
Color pasty state organosilicon electrically conductive ink.Wherein a=5, b=5, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 9000-11000mPa.s/25 DEG C.
Execute example 4
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 316 | 78.75% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.00% |
| 3 | Conductive black | 40.125 | 10% |
| 4 | Graphite powder | 40.125 | 10% |
| 5 | 0.2% chloroplatinic acid catalyst | 1 | 0.25% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=200, molecular weight about 15017) as shown in formula III is added to instead
Answer bottle, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.It is warming up to 100 DEG C, slowly
Drip 0.01 mole of structure hydrogeneous phenyl silicone oil (a=5, b=5, molecular weight about 1496.6) as shown in formula IV, within 4 hours, add, then
Insulation reaction 3 hours, completes reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl as shown in formula II embedding
Section silicone oil, weighs 316 grams, wherein a=5, b=5, m=200；Molecular weight about 31,531.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 316 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=200 as shown in formula II；
Molecular weight about 31,531) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
40.125 grams of conductive blacks and 40.125 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain
401.25 gram black paste organosilicon electrically conductive ink.Wherein a=5, b=5, m=200；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 8500-10000mPa.s/25 DEG C.
Embodiment 5
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 330 | 78.80% |
| 2 | Containing hydrogen silicone oil I | 4 | 0.96% |
| 3 | Conductive black | 20.94 | 5% |
| 4 | Graphite powder | 62.81 | 15% |
| 5 | 0.2% chloroplatinic acid catalyst | 1 | 0.24% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=200, molecular weight about 15017) as shown in formula III is added to instead
Answer bottle, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.It is warming up to 100 DEG C, slowly
Drip 0.01 mole of structure hydrogeneous phenyl silicone oil (a=10, b=10, molecular weight about 2858.8) as shown in formula IV, within 4 hours, add,
Insulation reaction 5 hours again, complete reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl as shown in formula II
Block silicone oil, weighs 330 grams, wherein a=10, b=10, m=200；Molecular weight about 32,893.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 330 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=10, b=10, m=as shown in formula II
200；Molecular weight about 32,893) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil (x=1, y=5, molecular weight as shown in formula I
About 568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then
Add, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
20.94 grams of conductive blacks and 62.81 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain
418.75 gram black paste organosilicon electrically conductive ink.Wherein a=10, b=10, m=200；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 9000-11000mPa.s/25 DEG C.
Embodiment 6
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 357 | 73.55% |
| 2 | Containing hydrogen silicone oil I | 6.04 | 1.24% |
| 3 | Conductive black | 24.27 | 5% |
| 4 | Graphite powder | 97.08 | 20% |
| 5 | 0.2% chloroplatinic acid catalyst | 1 | 0.21% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=200, molecular weight about 15017) as shown in formula III is added to instead
Answer bottle, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.It is warming up to 130 DEG C, slowly
Drip 0.01 mole of structure hydrogeneous phenyl silicone oil (a=20, b=20, molecular weight about 5583.4) as shown in formula IV, within 5 hours, add,
Insulation reaction 2 hours again, complete reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl as shown in formula II
Block silicone oil, weighs 357 grams, wherein a=20, b=20, m=200；Molecular weight about 35,617.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 357 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=20, b=20, m=as shown in formula II
200；Molecular weight about 35,617) and containing hydrogen silicone oil as shown in formula I of 6.04 grams of (about 0.006 mole) structures (x=2, y=10, point
Son amount about 1006, hydrogeneous 0.4%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.
It is subsequently adding, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, slowly add
Enter 24.27 grams of conductive blacks and 97.08 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain
485.4 grams of black paste organosilicon electrically conductive inks.Wherein a=20, b=20, m=200；X=2, y=10.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 10000-12000mPa.s/25 DEG C.
Embodiment 7
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 776 | 78.87% |
| 2 | Containing hydrogen silicone oil I | 9.59 | 0.97% |
| 3 | Conductive black | 98.39 | 10% |
| 4 | Graphite powder | 98.39 | 10% |
| 5 | 0.2% chloroplatinic acid catalyst | 1.5 | 0.16% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=500, molecular weight about 37264) as shown in formula III is added to instead
Answer bottle, add 2.5 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.It is warming up to 120 DEG C, slowly
0.01 mole of structure hydrogeneous phenyl silicone oil (a=10, b=10, molecular weight about 2858.8) as shown in formula IV of slow dropping, adds for 4 hours
Complete, then insulation reaction 5 hours, complete reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end ethylene as shown in formula II
Base block silicone oil, weighs 776 grams, wherein a=10, b=10, m=500；Molecular weight about 77,387.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 776 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=10, b=10, m=as shown in formula II
500；Molecular weight about 77,387) and containing hydrogen silicone oil as shown in formula I of 9.59 grams of (about 0.005 mole) structures (x=5, y=20, point
Son amount about 1918, hydrogeneous 0.37%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution
800rpm.It is subsequently adding, adds 1.5 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.?
After, it is slowly added into 98.39 grams of conductive blacks and 98.39 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution
2000rpm, obtains 983.86 grams of black paste organosilicon electrically conductive inks.Wherein a=10, b=10, m=500；X=5, y=20.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 9000-10500mPa.s/25 DEG C.
Embodiment 8
Organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 803 | 78.08% |
| 2 | Containing hydrogen silicone oil I | 17.73 | 1.72% |
| 3 | Conductive black | 51.42 | 5% |
| 4 | Graphite powder | 154.26 | 15% |
| 5 | 0.2% chloroplatinic acid catalyst | 2 | 0.19% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process is:
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=500, molecular weight about 37264) as shown in formula III is added to instead
Answer bottle, add 2 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.It is warming up to 120 DEG C, slowly
Drip 0.01 mole of structure hydrogeneous phenyl silicone oil (a=20, b=20, molecular weight about 5583.4) as shown in formula IV, within 6 hours, add,
Insulation reaction 6 hours again, complete reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl as shown in formula II
Block silicone oil, weighs 803 grams, wherein a=20, b=20, m=500；Molecular weight about 80,111.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 803 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=20, b=20, m=as shown in formula II
500；Molecular weight about 80,111) and containing hydrogen silicone oil as shown in formula I of 17.73 grams of (about 0.006 mole) structures (x=10, y=30,
Molecular weight about 2955, hydrogeneous 0.41%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution
800rpm.It is subsequently adding, adds 2 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally,
It is slowly added into 51.42 grams of conductive blacks and 154.26 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution
2000rpm, obtains 1028.4 grams of black paste organosilicon electrically conductive inks.Wherein a=20, b=20, m=500；X=10, y=
30。
The test result of this organosilicon electrically conductive ink is as follows: viscosity 11000-1300mPa.s/25 DEG C.
Comparative example 1
Comparative example 1 electrically conductive ink contains the 2-Butoxyethyl acetate solvent of 5%, organosilicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 69.39% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.65% |
| 3 | Conductive black | 11.5 | 4.75% |
| 4 | Graphite powder | 46 | 19% |
| 5 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.21% |
| 6 | 2-Butoxyethyl acetate | 12.1 | 5% |
| Add up to 100% |
(1) end-vinyl block silicone oil II preparation method: same as in Example 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
11.5 grams of conductive blacks and 46 grams of graphite powders, add 12.1 grams of glycol methyl ether acetates and be diluted, high-speed stirred mixing in 1 hour
Uniformly, agitation revolution 2000rpm, obtain 242.1 grams of black paste organosilicon electrically conductive inks.Wherein a=5, b=5, m=100；x
=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: solvent ≈ 5%；Viscosity 5000-7000mPa.s/25 DEG C.
Comparative example 2
Comparative example 2 electrically conductive ink uses common end-vinyl phenyl silicone oil replace end-vinyl block silicone oil II, have
Machine silicon conducting ink formulation:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl phenyl silicone oil | 168 | 73.04% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.74% |
| 3 | Conductive black | 11.5 | 5% |
| 4 | Graphite powder | 46 | 20% |
| 5 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.22% |
| Add up to 100% |
Organosilicon electrically conductive ink preparation process:
By 168 grams of end-vinyl phenyl silicone oil (phenyl content 5%, contents of ethylene 0.2%) and 4 grams, (about 0.007 rubs
You) and structure containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight about 568, hydrogeneous 0.53%) add in beaker, room temperature
Under, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.It is subsequently adding, adds 0.5 gram of chloroplatinic acid catalyst (0.2%
Isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into 11.5 grams of conductive blacks and 46 grams of graphite powders, adds 12.1
Gram glycol methyl ether acetate is diluted, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain 230 grams black
Color pasty state organosilicon electrically conductive ink.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 8500-10000mPa.s/25 DEG C.
Comparative example 3
Phenyl in end-vinyl block silicone oil II is replaced with methyl, organosilicon conductive oil by comparative example 3 electrically conductive ink
Ink formulations:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 161.8 | 72.97% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.8% |
| 3 | Conductive black | 11.09 | 5% |
| 4 | Graphite powder | 44.35 | 20% |
| 5 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.23% |
| Add up to 100% |
(1) end-vinyl block silicone oil II preparation method:
0.02 mole of structure vinyl-terminated silicone fluid (m=100, molecular weight about 7602) as shown in formula III is added to reaction
Bottle, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stirs.It is warming up to 120 DEG C, slowly drips
Add 0.01 mole of structure containing hydrogen silicone oil (a=0, b=10, molecular weight about 875.8) as shown in formula IV, within 2 hours, add, then insulation is anti-
Answer 4 hours, complete reaction.It is cooled to less than 40 DEG C, obtains 0.01 mole of structure end-vinyl block silicone oil as shown in formula II,
Weigh 161.8 grams, wherein a=0, b=10, m=100；Molecular weight about 16,080.Outward appearance is colourless oil liquid.
(2) organosilicon electrically conductive ink preparation process:
By 161.8 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=0, b=10, m=as shown in formula II
100；Molecular weight about 16,080) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil (x=1, y=5, molecular weight as shown in formula I
About 568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then
Add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
11.09 grams of conductive blacks and 44.35 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain
221.7 grams of black paste organosilicon electrically conductive inks.Wherein a=0, b=10, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 7000-9000mPa.s/25 DEG C.
Comparative example 4
Without graphite powder in comparative example 4 electrically conductive ink, only use conductive black as conductive material, organosilicon electrically conductive ink
Formula:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 77.91% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.86% |
| 3 | Conductive black | 43.125 | 20% |
| 4 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.23% |
| Add up to 100% |
(1) end-vinyl block silicone oil II preparation method: same as in Example 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
43.125 grams of conductive blacks, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtaining 215.6 grams of black paste has
Machine silicon electrically conductive ink.Wherein a=5, b=5, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 9000-11000mPa.s/25 DEG C.
Comparative example 5
Without conductive black in comparative example 5 electrically conductive ink, only use graphite powder as conductive material, organosilicon electrically conductive ink
Formula:
| Numbering | Material name | Consumption (gram) | Account for percentage by weight |
| 1 | End-vinyl block silicone oil II | 168 | 68.18% |
| 2 | Containing hydrogen silicone oil I | 4 | 1.62% |
| 3 | Graphite powder | 73.93 | 30% |
| 4 | 0.2% chloroplatinic acid catalyst | 0.5 | 0.2% |
| Add up to 100% |
(1) end-vinyl block silicone oil II preparation method: same as in Example 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures end-vinyl block silicone oil (a=5, b=5, m=100 as shown in formula II；
Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures containing hydrogen silicone oil as shown in formula I (x=1, y=5, molecular weight is about
568, hydrogeneous 0.53%) add in beaker, under room temperature, use overhead type stirrer mix homogeneously, agitation revolution 800rpm.Then add
Enter, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix homogeneously.Finally, it is slowly added into
73.93 grams of graphite powders, 1 hour mix homogeneously of high-speed stirred, agitation revolution 2000rpm, obtain 246.4 grams of black paste organosilicons
Electrically conductive ink.Wherein a=5, b=5, m=100；X=1, y=5.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 6000-8000mPa.s/25 DEG C.
Application Example
Embodiment 9
All electrically conductive inks are fabricated to conducting sample, testing conductive performance, washing fastness, folding quality after solidification crosslinking.
1, sample making:
Use silk-screen printing technique, with 200 mesh silk screen printings, on the cloth of 200mm × 100mm printing 120mm ×
The coating of 60mm, then 150 DEG C of crosslinkings 15 minutes that are heating and curing, obtains conducting sample.Embodiment 1-5 uses cotton, implements
Example 6,7 uses polyester-mixed cotton cloth (50/50), and embodiment 8 uses woven dacron, and comparative example 1-5 uses cotton.
2, sheet resistance test
The double electrical measurement four-point probe of RTS-9 is used to measure.
3, washable method of testing
Testing standard: BS EN ISO 6330:2012
Washing procedure: 4N
Sample gross weight: dry weight 2 kilograms (when weight is less than 2 kilograms, adds white cotton and supplies weight)
Washing machine: roller washing machine
Water temperature: 40 DEG C
Detergent: detergent A (commercially available non-phosphide detergent), each 20 grams
Washing process: wash 15 minutes, rinses four times, 3,3,2,2 minutes respectively, dries one time 5 minutes.Wash knot every time
Will dry with dryer after bundle.1 complete washing process=washing 1 time+dry 1 time
After washing 50 times, measure sheet resistance value.
4, the method for testing of fold resistant performance
Instrument: the HT-1063 machine of resistance to bending and unbending test
Counterweight: 200 grams of counterweights；
Folding rate: 60 beats/min
Sample is drawn three parallel lines in a vertical direction, is spaced 10mm.Sample is clipped on fixture, accurately clip to centre
Those parallel lines, hang the counterweight of 200 gram masses below sample.
The HT-1063 machine of resistance to bending and unbending test is set to 3000 times, then runs, carry out 180 ° of foldings (-90 °-+90 °), reach
After predetermined number of times, machine is out of service, takes off sample, the sheet resistance value at those parallel lines two ends in the middle of test.
The electric conductivity test result of table 1 organosilicon electrically conductive ink
The printing conductive coating sheet resistance of the present invention is in 103-104Ω/sq scope, prints on the textile and heats
After solidification crosslinking, coating uniform, soft, flexible, it is suitable for use in the purposes such as antistatic.And comparative example 1 conductive coating is to the greatest extent
Tube-surface resistance is in 103-104Ω/sq scope, but coating Boardy Feeling, poor flexibility；And comparative example 4 and 5 use conduction charcoals
One in black or graphite powder is as conductive material, and electric conductivity is the most poor, and sheet resistance is in 105-106Ω/sq scope.
The washable test result of table 2 organosilicon electrically conductive ink
∞ represents the resistance range beyond 200M Ω, it is possible to understand that infinite, non-conductive.
∞*Represent infinity.
After 50 times are washed, the conductive coating of the present invention stands intact, and sheet resistance is still in 103-104Ω/sq model
Enclosing, resistance change rate is less than ± 20%, shows that coating washing resistance performance is good.And comparative example conductive coating is the most washable, contrast
Example 1 wash 50 times after coating shedding, expose cloth；Comparative example 2,3 washs coating damage after 50 times, partial exfoliation；Comparative example 4 He
After 5 washings, resistance change rate is considerably beyond ± 20%, washing fastness poor (seeing Fig. 2 a-c).
The fold resistant test result of table 3 organosilicon electrically conductive ink
After 3000 times fold, the conductive coating surface of the present invention has no folding line, and sheet resistance is still in 103-104Ω/
Sq scope, resistance change rate is less than ± 20%, shows that coating fold resistant performance is good.And comparative example 1,2,4,5 conductive coating folding
Poststack resistance change rate, considerably beyond ± 20%, shows that obvious folding line even occur in fold resistant poor performance, comparative example 1, the most right
Ratio 3 fold resistant better performances (sees Fig. 3 a-c).
The application test data of table 1,2,3 show, the organosilicon electrically conductive ink of the present invention has the advantage that
1, excellent washing resistance performance: on the textile after printing, is amenable to 50 washings of washing machine and conductive coating is complete
Good lossless, after washing, coated conductive change is less than ± 20%.
2, prominent fold resistant performance: on the textile after printing, be amenable to 180 ° folding, and conductive coating does not goes out
Existing slight crack, after folding 3000 times, coated conductive change is less than ± 20%.
3, conduct electricity very well: using the conductive material such as white carbon black and graphite powder, sheet resistance is up to 103-105Ω/sq (conduction
Coating layer thickness 30 μm), lower than conventional antistatic printing ink.
4, impressionability can be good: available conventional screen printing mode is in textile surface printing, very easy to use.
Claims (9)
1. the organosilicon electrically conductive ink of a wash resistant fold resistant, it is characterised in that: by weight percentage, electrically conductive ink by
The polymerizable organosilicon monomer of 60-85%, 10-35% conductive material and 0.01-5% catalyst are jointly compounding to be formed；
Wherein, polymerizable organosilicon monomer is collectively constituted by end-vinyl block silicone oil II and containing hydrogen silicone oil I；Conductive material is by conducting electricity
White carbon black and graphite powder collectively constitute；Catalyst is the aqueous isopropanol of chloroplatinic acid；
In formula:
A=5-20, b=5-20, m=100-500；X=1-10；Y=5-30；
Wherein, the preparation reaction of end-vinyl block silicone oil II is as follows:
In formula: a=5-20, b=5-20, m=100-500；
Hydrogeneous phenyl silicone oil IV is reacted 2-20 hour at 80-150 DEG C with vinyl-terminated silicone fluid III in the presence of a catalyst, generates end
Ethylene based block silicone oil II；
Wherein, hydrogeneous phenyl silicone oil IV is 1:2-3 with the mol ratio of vinyl-terminated silicone fluid III；The addition of catalyst is conductive oil
The 0.01-5% of ink weight；Catalyst is the aqueous isopropanol of chloroplatinic acid.
2. according to the organosilicon electrically conductive ink of the wash resistant fold resistant described in claim 1, it is characterised in that: percentage by weight
Than meter, electrically conductive ink is compounded jointly by the polymerizable organosilicon monomer of 65-80%, 19-34% conductive material and 0.1-1% catalyst
Form.
3. according to the organosilicon electrically conductive ink of the wash resistant fold resistant described in claim 1, it is characterised in that: described end-vinyl
The preparation of block silicone oil II be hydrogeneous phenyl silicone oil IV in the presence of a catalyst with vinyl-terminated silicone fluid III 100-130 DEG C of reaction
3-12 hour, generate end-vinyl block silicone oil II；
Wherein, hydrogeneous phenyl silicone oil IV is 1:2 with the mol ratio of vinyl-terminated silicone fluid III；The addition of catalyst is electrically conductive ink
The 0.1-1% of weight.
4. the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 1, it is characterised in that: described end-vinyl is embedding
In section silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of reactive hydrogen is 1:1-20.
5. the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 4, it is characterised in that: described end-vinyl is embedding
In section silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of reactive hydrogen is 1:1-5.
6. the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 1, it is characterised in that: in described conductive material
The weight ratio of conductive black and graphite powder is 1:1-10.
7. the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 6, it is characterised in that: in described conductive material
The weight ratio of conductive black and graphite powder is 1:1-7.
8. the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 1, it is characterised in that: described graphite powder is pure
The high-purity graphite powder of degree >=99.85%, its particle mean size≤30 μm.
9. the application of the organosilicon electrically conductive ink of the wash resistant fold resistant as described in claim 1, it is characterised in that: described washable
The organosilicon electrically conductive ink washing fold resistant is applied in textile antistatic or conducting channel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0545002A1 (en) * | 1991-11-21 | 1993-06-09 | Kose Corporation | Silicone polymer, paste-like composition and water-in-oil type cosmetic composition comprising the same |
| CN102191012A (en) * | 2011-03-22 | 2011-09-21 | 上海本诺电子材料有限公司 | Solvent-free monocomponent organosilicon conducting resin used in LEDs and preparation method thereof |
| CN102516930A (en) * | 2011-12-13 | 2012-06-27 | 烟台德邦科技有限公司 | High temperature curing monocomponent heat-conduction flame-retardation electronic pouring sealant and preparation method thereof |
| CN103865272A (en) * | 2014-03-20 | 2014-06-18 | 株洲时代新材料科技股份有限公司 | Organic silicon impedance glue and preparation method thereof |
-
2014
- 2014-12-22 CN CN201410806529.2A patent/CN104530833B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0545002A1 (en) * | 1991-11-21 | 1993-06-09 | Kose Corporation | Silicone polymer, paste-like composition and water-in-oil type cosmetic composition comprising the same |
| CN102191012A (en) * | 2011-03-22 | 2011-09-21 | 上海本诺电子材料有限公司 | Solvent-free monocomponent organosilicon conducting resin used in LEDs and preparation method thereof |
| CN102516930A (en) * | 2011-12-13 | 2012-06-27 | 烟台德邦科技有限公司 | High temperature curing monocomponent heat-conduction flame-retardation electronic pouring sealant and preparation method thereof |
| CN103865272A (en) * | 2014-03-20 | 2014-06-18 | 株洲时代新材料科技股份有限公司 | Organic silicon impedance glue and preparation method thereof |
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