CN104530833A - Organosilicone conductive ink - Google Patents

Organosilicone conductive ink Download PDF

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Publication number
CN104530833A
CN104530833A CN201410806529.2A CN201410806529A CN104530833A CN 104530833 A CN104530833 A CN 104530833A CN 201410806529 A CN201410806529 A CN 201410806529A CN 104530833 A CN104530833 A CN 104530833A
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CN
China
Prior art keywords
silicone oil
electrically conductive
organosilicon
conductive ink
vinyl
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CN201410806529.2A
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CN104530833B (en
Inventor
魏峰
董仕晋
刘歌
王瑛
刘冬雪
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Shenyang Research Institute of Chemical Industry Co Ltd
Sinochem Corp
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Shenyang Research Institute of Chemical Industry Co Ltd
Sinochem Corp
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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
    • 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
    • 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
    • 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 & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention belongs to the technical fields of polymer and conductive ink, and relates to organosilicone conductive ink. The conductive ink is formed by compounding an organosilicone polymerization monomer, a conductive material and a catalyst, wherein the organosilicone polymerization monomer is composed of vinyl-terminated block silicone oil II defined in the description and hydrogen-containing silicone oil I defined in the description, wherein a is equal to 5-20, b is equal to 5-20 and m is equal to 100-500; x is equal to 1-10 and y is equal to 5-30; the conductive material is composed of conductive carbon black and graphite powder, and the catalyst is chloroplatinic acid.

Description

A kind of organosilicon electrically conductive ink
Technical field
The invention belongs to polymer and electrically conductive ink technical field, be specifically related to a kind of organosilicon electrically conductive ink.
Background technology
Electrically conductive ink good conductivity, cost are low, advantages of nontoxic raw materials or low toxicity, high, easy to use with base material binding strength, and progressively Substitute For Partial metallic circuit, in field widespread uses such as photovoltaic industry, printed wiring, biosensor, electromagnetic shielding material, ID card, RFID antenna.Electrically conductive ink starts to use at emerging fields such as intelligent textiles in recent years, for the purposes such as printing electrically conductive circuits and antistatic coating, but this conducting channel and antistatic coating not wash resistant, non-fold resistant, work-ing life is short, and impact popularizes.In order to overcome above-mentioned shortcoming, needing to improve conducting ink formulation, to improve washable, folding quality when it is applied on the textile, increasing the service life.
Current commercially available electrically conductive ink kind is a lot, and such as common Acheson423SS, CH-8 etc. have excellent conductivity, and in PET film, printed coating can bend 180-360 °, but can not be folding.By these electrically conductive ink printings on the textile, conductive coating is wash resistant not, also not fold resistant.
Iida Kazani etc. are at Fibres & Textiles in Eastern Europe, 2012, mention in 20 (1): 57-63, one deck silver electrically conductive ink is smeared at textile surface, measure coating washing fastness, wash 20 times in washing machine after, the conductive coating of sample segment comes off, the resistance value of all the other samples increases 60-1500 doubly, and all samples is not washable.If at surface-coated one deck protective polyurethane layer of conductive coating; then sample washing fastness increases, and after washing 20 times, has the resistance value of two samples only to improve 10-25% in washing machine; can think washable 20 times, but also there is a big difference for the standard of this and washable 50 times.
Up to the present, there is not yet can use on the textile, can washable 50 times, the bibliographical information of the folding electrically conductive ink of ability 180 °.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of organosilicon electrically conductive ink of wash resistant fold resistant is provided.
The technical solution used in the present invention is for achieving the above object:
An organosilicon electrically conductive ink for wash resistant fold resistant, by weight percentage, electrically conductive ink by 60-85% polymerizable organosilicon monomer, 10-35% electro-conductive material and 0.01-5% catalyzer is jointly composite forms;
Wherein, polymerizable organosilicon monomer is made up of jointly end-vinyl block silicone oil II and containing hydrogen silicone oil I; Electro-conductive material is made up of jointly graphitized carbon black and Graphite Powder 99; Catalyzer is the aqueous isopropanol of Platinic chloride;
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 by 65-80% polymerizable organosilicon monomer, 19-34% electro-conductive material and 0.1-1% catalyzer is jointly composite forms.
The preparation feedback 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 reacts 2-20 hour with vinyl-terminated silicone fluid III at 80-150 DEG C in the presence of a catalyst, generates 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 add-on of catalyzer is the 0.01-5% of electrically conductive ink weight; Catalyzer is the aqueous isopropanol of Platinic chloride.
The preparation of end-vinyl block silicone oil II preferably, hydrogeneous phenyl silicone oil IV react 3-12 hour with vinyl-terminated silicone fluid III at 100-130 DEG C in the presence of a catalyst, generation 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 add-on of catalyzer is the 0.1-1% of electrically conductive ink weight.
In described end-vinyl block silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of active hydrogen is 1:1-20.Containing hydrogen silicone oil I partly by commercially available acquisition, also can be prepared 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 active hydrogen is 1:1-5.
In described electro-conductive material, the weight ratio of graphitized carbon black and Graphite Powder 99 is 1:1-10.Graphitized carbon black and Graphite Powder 99 can by commercially available acquisitions.
Preferably, in described electro-conductive material, the weight ratio of graphitized carbon black and Graphite Powder 99 is 1:1-7.
Described Graphite Powder 99 is the high-purity graphite powder of purity >=99.85%, its mean particle size≤30 μm.
An application for the organosilicon electrically conductive ink of wash resistant fold resistant, the organosilicon electrically conductive ink of described wash resistant fold resistant is applied in the antistatic or conducting channel of textiles.
The advantage that the present invention has: organosilicon electrically conductive ink of the present invention is printed on the base materials such as textiles, after curing cross-linked, form netted silicone resin coating, good with base material binding strengths such as textiless, feel is very soft, can stand folding and not damage, washing resistance performance is better than the electrically conductive ink using polyacrylic resin far away.
The organosilicon electrically conductive ink of wash resistant fold resistant of the present invention is used for the purposes such as the antistatic or conducting channel of textiles.Because its electroconductibility is relatively good, during conductive coating thickness 30 microns, surface resistivity is in 10 3-10 4Ω/sq scope, print on the textile and be heating and curing crosslinked after, coating uniform, soft, flexible.If use the Graphite Powder 99 that particle is less, just can make thinner by printed coating thickness in application process, this promotes advantageously produce market.
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 are cross-linked to form tridimensional network through being heating and curing, the washable silicone resin coating of resistance to fold-type obtained.Coating and fiber binding strength high, there is organosilyl distinctive flexibility; And the phenyl silica block in molecule effectively can promote coating hardness, give scratch-resistant, wear resisting property that coating is special, the friction repeatedly of inner tank of washing machine can be born when washing, and the friction repeatedly of clothes-drying machine inner core and shock when drying, ensure that coating is repeatedly washed and do not damage.When electrically conductive ink of the present invention is applied on the textile, conductive coating can be washed with washing machine, can be folding, coating long service life.Specifically:
1, wash resistant: on the textile after printing, can stand washing machine 50 times washing and conductive coating stands intact, after washing coated conductive change be no more than ± 20%.
2, fold resistant: on the textile after printing, can stand 180 ° folding, and there is not slight crack in conductive coating, after folding 3000 times coated conductive change be no more than ± 20%.
3, conductivity: use the electro-conductive material such as carbon black and Graphite Powder 99, surface resistivity can reach 10 3-10 5Ω/sq (conductive coating thickness 30 μm).
4, impressionability energy: the screen printing mode of available routine 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 of 50 front and back for conducting sample that the embodiment of the present invention provides, and wherein a is sample before adopting conductive coating of the present invention washing, b is sample after adopting conductive coating of the present invention to wash 50 times, c adopts comparative example conductive coating to wash the sample after 50 times.
Fig. 3 for conducting sample that the embodiment of the present invention provides fold before and after design sketch, wherein a be adopt that conductive coating of the present invention folds front sample, b be adopt conductive coating folded swatch of the present invention, c is sample after adopting comparative example conductive coating to fold.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the invention will be further elaborated, but the present invention is only limitted to this absolutely not.
Polymerizable organosilicon monomer of the present invention is made up of jointly end-vinyl block silicone oil II and containing hydrogen silicone oil I, if in order to reduce costs, end-vinyl block silicone oil II is replaced by end-vinyl phenyl silicone oil common on market, then washing fastness obviously declines, do not reach the requirement of washable 50 times, folding quality also declines.Equally, in order to reduce costs object, replace end-vinyl block silicone oil II with the end-vinyl methyl-silicone oil not containing phenyl, then coating washing fastness is very poor equally, and coating is damaged after repetitive scrubbing, does not reach the requirement of washable 50 times.
Electro-conductive material of the present invention is made up of jointly graphitized carbon black and Graphite Powder 99, and in order to improve the conductivity of organosilicon electrically conductive ink, the weight ratio of the two is 1:1-10, preferred 1:1-7; Ratio is too high or too low, and electroconductibility all obviously declines.If be used alone graphitized carbon black or Graphite Powder 99, then electroconductibility is poorer.In order to promote conductivity, Graphite Powder 99 used is the high-purity graphite powder of purity >=99.85%, and the Graphite Powder 99 poorly conductive that purity is low should not adopt.Mean particle size≤30 μm of Graphite Powder 99, are just not easy network blocking when using the mode printing conductive inks such as silk screen printing like this.Graphitized carbon black comprises the various model graphitized carbon blacks that market can have been bought, pay the utmost attention to the graphitized carbon black that good conductivity, granularity are thin, the common trade mark comprises BP2000, VXC-72R, VXC-72, AS-300J, EC-600JD, EC-300J, 3350B, T-90 etc.
Catalyzer is Platinic chloride, and can be mixed with platinum acid chloride solution in advance for convenience of using, conventional is isopropyl alcohol solution of chloroplatinic acid, and concentration is 0.01-5% (w/w), preferred 0.1-1%.Use during catalyzer and want appropriate, add the period of storage that excessive catalyzer can shorten electrically conductive ink, the electrically conductive ink quality guaranteed period of the present invention is room temperature about 1 year, within after adding excess catalyst, the period of storage of electrically conductive ink can shorten to 6 months.High reactivity amines catalyst should not use, otherwise the period of storage of electrically conductive ink can be very short, affects its commercial value.
The organosilicon electrically conductive ink of described wash resistant fold resistant is applied in the antistatic or conducting channel of textiles.Organosilicon electrically conductive ink of the present invention is different from commercially available electrically conductive ink, commercially available electrically conductive ink adds a certain amount of solvent usually, for dissolving resin and increase mobility, and electro-conductive material is uniformly dispersed, about solvent in Acheson423SS, CH-8 accounts for the half of gross weight, but organosilicon electrically conductive ink of the present invention does not allow to add too much solvent.Such as quantity of solvent reaches 5%, will have influence on the curing cross-linked effect of organosilane monomer, and coating is washable all significantly to be reduced with folding quality.
Raw material used in the embodiment of the present invention all has commercially available, also can prepare according to the mode known by those skilled in the art.C in formula 6h 5-represent phenyl.
Standard method test (BS EN ISO6330:2012) is adopted to the washing fastness of organosilicon electrically conductive ink of the present invention.
Fold resistant performance adopts the domestic HT-1063 machine of resistance to bending and unbending test to 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%
Graphitized carbon black ... industrial goods
Graphite Powder 99 ... purity >=99.85%, mean particle size≤30 μm
2-Butoxyethyl acetate ... industrial goods, 99%
Platinic chloride ... ... ... ... industrial goods, 99%
Virahol ... ... ... ... .. analytical pure, 99%
0.2% chloroplatinic acid catalyst (2 grams of Platinic chlorides are dissolved in 998 grams of Virahols, are made into 0.2% solution)
The reference preparation method of hydrogeneous phenyl silicone oil:
In four mouthfuls of round-bottomed flasks that agitator, thermometer, reflux condensing tube are housed, add tetramethyldihydrogendisiloxane and the octamethylcyclotetrasiloxane of requirement, desired reaction temperature (such as 50-80 DEG C) is warming up under stirring, add a small amount of vitriol oil, insulation reaction 2-4 hour, then add the octaphenylcyclotetrasiloxane of requirement, then react 2-8 hour.Cool to room temperature, with anhydrous sodium carbonate neutralization, solids removed by filtration thing.Filtrate with water pump-0.095MPa vacuum removal low-boiling-point substance, namely obtains hydrogeneous phenyl silicone oil in 120-150 DEG C.
Preparation embodiment
Embodiment 1
Organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 73.04％
2 Containing hydrogen silicone oil I 4 1.74％
3 Graphitized carbon black 11.5 5％
4 Graphite Powder 99 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 silicone resin being heating and curing in cross-linking process, and reaction formula 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=100, molecular weight about 7602) shown in III, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 120 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=5, b=5, molecular weight about 1496.6), within 2 hours, add, then insulation reaction 4 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 11.5 grams of graphitized carbon blacks and 46 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 230 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: viscosity 8000-10000mPa.s/25 DEG C.
Embodiment 2
Organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 67.2％
2 Containing hydrogen silicone oil I 4 1.6％
3 Graphitized carbon black 10 4％
4 Graphite Powder 99 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: identical with embodiment 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 10 grams of graphitized carbon blacks and 67.5 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 250 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: viscosity 5000-7000mPa.s/25 DEG C.
Embodiment 3
Organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 74.78％
2 Containing hydrogen silicone oil I 4 1.78％
3 Graphitized carbon black 17.97 8％
4 Graphite Powder 99 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: identical with embodiment 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 17.97 grams of graphitized carbon blacks and 33.7 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 224.67 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: viscosity 9000-11000mPa.s/25 DEG C.
Execute example 4
Organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 316 78.75％
2 Containing hydrogen silicone oil I 4 1.00％
3 Graphitized carbon black 40.125 10％
4 Graphite Powder 99 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=200, molecular weight about 15017) shown in III, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 100 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=5, b=5, molecular weight about 1496.6), within 4 hours, add, then insulation reaction 3 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=5, b=5, the m=200 shown in II; Molecular weight about 31,531) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 40.125 grams of graphitized carbon blacks and 40.125 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 401.25 grams of black paste organosilicon electrically conductive inks.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 weight percent
1 End-vinyl block silicone oil II 330 78.80％
2 Containing hydrogen silicone oil I 4 0.96％
3 Graphitized carbon black 20.94 5％
4 Graphite Powder 99 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=200, molecular weight about 15017) shown in III, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 100 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=10, b=10, molecular weight about 2858.8), within 4 hours, add, then insulation reaction 5 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=10, b=10, the m=200 shown in II; Molecular weight about 32,893) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 20.94 grams of graphitized carbon blacks and 62.81 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 418.75 grams of black paste organosilicon electrically conductive inks.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 weight percent
1 End-vinyl block silicone oil II 357 73.55％
2 Containing hydrogen silicone oil I 6.04 1.24％
3 Graphitized carbon black 24.27 5％
4 Graphite Powder 99 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=200, molecular weight about 15017) shown in III, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 130 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=20, b=20, molecular weight about 5583.4), within 5 hours, add, then insulation reaction 2 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=20, b=20, the m=200 shown in II; Molecular weight about 35,617) and 6.04 grams of (about 0.006 mole) structures such as formula containing hydrogen silicone oil (x=2, the y=10 shown in I, molecular weight about 1006, hydrogeneous 0.4%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 24.27 grams of graphitized carbon blacks and 97.08 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 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 weight percent
1 End-vinyl block silicone oil II 776 78.87％
2 Containing hydrogen silicone oil I 9.59 0.97％
3 Graphitized carbon black 98.39 10％
4 Graphite Powder 99 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=500, molecular weight about 37264) shown in III, adds 2.5 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 120 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=10, b=10, molecular weight about 2858.8), within 4 hours, add, then insulation reaction 5 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=10, b=10, the m=500 shown in II; Molecular weight about 77,387) and 9.59 grams of (about 0.005 mole) structures such as formula containing hydrogen silicone oil (x=5, the y=20 shown in I, molecular weight about 1918, hydrogeneous 0.37%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 1.5 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 98.39 grams of graphitized carbon blacks and 98.39 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, 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 weight percent
1 End-vinyl block silicone oil II 803 78.08％
2 Containing hydrogen silicone oil I 17.73 1.72％
3 Graphitized carbon black 51.42 5％
4 Graphite Powder 99 154.26 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=500, molecular weight about 37264) shown in III, adds 2 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 120 DEG C, slowly drip 0.01 mole of structure such as formula phenyl silicone oil hydrogeneous shown in IV (a=20, b=20, molecular weight about 5583.4), within 6 hours, add, then insulation reaction 6 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in II, weigh 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 such as formula end-vinyl block silicone oil (a=20, b=20, the m=500 shown in II; Molecular weight about 80,111) and 17.73 grams of (about 0.006 mole) structures such as formula containing hydrogen silicone oil (x=10, the y=30 shown in I, molecular weight about 2955, hydrogeneous 0.41%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 2 grams of chloroplatinic acid catalysts (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 51.42 grams of graphitized carbon blacks and 154.26 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, 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
Containing the 2-Butoxyethyl acetate solvent of 5% in comparative example 1 electrically conductive ink, organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 69.39％
2 Containing hydrogen silicone oil I 4 1.65％
3 Graphitized carbon black 11.5 4.75％
4 Graphite Powder 99 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: identical with embodiment 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 11.5 grams of graphitized carbon blacks and 46 grams of Graphite Powder 99s, add 12.1 grams of glycol methyl ether acetates and dilute, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 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
Common end-vinyl phenyl silicone oil is used to replace end-vinyl block silicone oil II, organosilicon conducting ink formulation in comparative example 2 electrically conductive ink:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl phenyl silicone oil 168 73.04％
2 Containing hydrogen silicone oil I 4 1.74％
3 Graphitized carbon black 11.5 5％
4 Graphite Powder 99 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 contents 5%, contents of ethylene 0.2%) and 4 grams of (about 0.007 mole) structures such as formula the containing hydrogen silicone oil (x=1 shown in I, y=5, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 11.5 grams of graphitized carbon blacks and 46 grams of Graphite Powder 99s, add 12.1 grams of glycol methyl ether acetates and dilute, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 230 grams of black paste organosilicon electrically conductive inks.
The test result of this organosilicon electrically conductive ink is as follows: viscosity 8500-10000mPa.s/25 DEG C.
Comparative example 3
In comparative example 3 electrically conductive ink, the phenyl in end-vinyl block silicone oil II is replaced with methyl, organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 161.8 72.97％
2 Containing hydrogen silicone oil I 4 1.8％
3 Graphitized carbon black 11.09 5％
4 Graphite Powder 99 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 is added to reaction flask such as formula the vinyl-terminated silicone fluid (m=100, molecular weight about 7602) shown in III, adds 1 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), stir.Be warming up to 120 DEG C, slowly drip 0.01 mole of structure such as formula containing hydrogen silicone oil shown in IV (a=0, b=10, molecular weight about 875.8), within 2 hours, add, then insulation reaction 4 hours, complete reaction.Be cooled to less than 40 DEG C, obtain 0.01 mole of structure such as formula the end-vinyl block silicone oil shown in 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 such as formula end-vinyl block silicone oil (a=0, b=10, the m=100 shown in II; Molecular weight about 16,080) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 11.09 grams of graphitized carbon blacks and 44.35 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 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
Not graphitiferous powder in comparative example 4 electrically conductive ink, only uses graphitized carbon black as electro-conductive material, organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 77.91％
2 Containing hydrogen silicone oil I 4 1.86％
3 Graphitized carbon 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: identical with embodiment 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 43.125 grams of graphitized carbon blacks, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 215.6 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: viscosity 9000-11000mPa.s/25 DEG C.
Comparative example 5
Not containing graphitized carbon black in comparative example 5 electrically conductive ink, only use Graphite Powder 99 as electro-conductive material, organosilicon conducting ink formulation:
Numbering Material name Consumption (gram) Account for weight percent
1 End-vinyl block silicone oil II 168 68.18％
2 Containing hydrogen silicone oil I 4 1.62％
3 Graphite Powder 99 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: identical with embodiment 1.
(2) organosilicon electrically conductive ink preparation process:
By 168 grams of (about 0.01 mole) structures such as formula end-vinyl block silicone oil (a=5, b=5, the m=100 shown in II; Molecular weight about 16,701) and 4 grams of (about 0.007 mole) structures such as formula containing hydrogen silicone oil (x=1, the y=5 shown in I, molecular weight about 568, hydrogeneous 0.53%) add in beaker, under room temperature, mix with overhead type stirrer, agitation revolution 800rpm.Then add, add 0.5 gram of chloroplatinic acid catalyst (0.2% isopropyl alcohol solution of chloroplatinic acid, w/w), mix.Finally, slowly add 73.93 grams of Graphite Powder 99s, high-speed stirring mixes for 1 hour, agitation revolution 2000rpm, obtains 246.4 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: viscosity 6000-8000mPa.s/25 DEG C.
Application Example
Embodiment 9
All electrically conductive inks are made into conducting sample, testing conductive performance, washing fastness, folding quality after curing cross-linked.
1, sample making:
Adopt silk-screen printing technique, with 200 order silk screen printings, the cloth of 200mm × 100mm is printed the coating of 120mm × 60mm, be then heating and curing crosslinked 15 minutes at 150 DEG C, obtain conducting sample.Embodiment 1-5 uses cotton, and embodiment 6,7 uses polyester-mixed cotton cloth (50/50), and embodiment 8 uses woven dacron, and comparative example 1-5 uses cotton.
2, surface resistivity test
The two electrical measurement four-point probe of RTS-9 is used to measure.
3, washable testing method
Testing standard: BS EN ISO 6330:2012
Washing procedure: 4N
Sample gross weight: dry weight 2 kilograms (during under weight 2 kilograms, add white cotton and supply weight)
Washing machine: roller washing machine
Water temperature: 40 DEG C
Washing composition: washing composition A (commercially available non-phosphide detergent), each 20 grams
Washing process: wash 15 minutes, rinsing four times, 3,3,2,2 minutes respectively, dries one time 5 minutes.All dry with clothes-drying machine after each washing terminates.1 complete washing process=washing 1 time+dry 1 time
After washing 50 times, surface measurements resistance value.
4, the testing method 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 draws three parallel lines by vertical direction, interval 10mm.Sample is clipped on fixture, accurately clip to those parallel lines middle, below sample, hang the counterweight of 200 gram masses.
The HT-1063 machine of resistance to bending and unbending test is set to 3000 times, then runs, carry out 180 ° folding (-90 °-+90 °), after reaching 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 electroconductibility test result of table 1 organosilicon electrically conductive ink
Printing conductive coating surface resistivity of the present invention is in 10 3-10 4Ω/sq scope, print on the textile and be heating and curing crosslinked after, coating uniform, soft, flexible, be suitable for use in the purposes such as antistatic.Although and comparative example 1 conductive coating surface resistivity is in 10 3-10 4Ω/sq scope, but coating Boardy Feeling, poor flexibility; And comparative example 4 and 5 use one in graphitized carbon blacks or Graphite Powder 99 as electro-conductive material, conductivity is obviously poor, and surface resistivity is in 10 5-10 6Ω/sq scope.
The washable test result of table 2 organosilicon electrically conductive ink
∞ represents the range that resistance exceeds 200M Ω, is appreciated that infinite, non-conductive.
∞ *represent infinity.
After 50 washings, conductive coating of the present invention stands intact, and surface resistivity is still in 10 3-10 4Ω/sq scope, resistance change rate is no more than ± and 20%, show that coating washing resistance performance is good.And comparative example conductive coating is not washable, coating shedding after comparative example 1 washs 50 times, exposes cloth; Coating damage after comparative example 2,3 washs 50 times, partial exfoliation; Comparative example 4 and 5 washs rear resistance change rate considerably beyond ± 20%, washing fastness difference (see Fig. 2 a-c).
The fold resistant test result of table 3 organosilicon electrically conductive ink
After 3000 times folding, conductive coating surface of the present invention has no folding line, and surface resistivity is still in 10 3-10 4Ω/sq scope, resistance change rate is no more than ± and 20%, show that coating fold resistant performance is good.And the folding rear resistance change rate of comparative example 1,2,4,5 conductive coating is considerably beyond ± 20%, showing fold resistant poor performance, even there is obvious folding line in comparative example 1, only has comparative example 3 fold resistant better performances (see Fig. 3 a-c).
Table 1,2, the application testing data of 3 show, organosilicon electrically conductive ink tool of the present invention has the following advantages:
1, excellent washing resistance performance: on the textile after printing, can stand washing machine 50 washings and conductive coating stands intact, after washing coated conductive change be no more than ± 20%.
2, outstanding fold resistant performance: on the textile after printing, can stand 180 ° folding, and there is not slight crack in conductive coating, after folding 3000 times coated conductive change be no more than ± 20%.
3, conduct electricity very well: use the electro-conductive material such as carbon black and Graphite Powder 99, surface resistivity can reach 10 3-10 5Ω/sq (conductive coating thickness 30 μm) is lower than conventional antistatic printing ink.
4, impressionability can be good: the screen printing mode of available routine is in textile surface printing, very easy to use.

Claims (10)

1. an organosilicon electrically conductive ink for wash resistant fold resistant, is characterized in that: by weight percentage, electrically conductive ink by 60-85% polymerizable organosilicon monomer, 10-35% electro-conductive material and 0.01-5% catalyzer is jointly composite forms;
Wherein, polymerizable organosilicon monomer is made up of jointly end-vinyl block silicone oil II and containing hydrogen silicone oil I; Electro-conductive material is made up of jointly graphitized carbon black and Graphite Powder 99; Catalyzer is the aqueous isopropanol of Platinic chloride;
In formula:
a＝5-20，b＝5-20，m＝100-500；x＝1-10；y＝5-30。
2., according to the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 1, it is characterized in that: by weight percentage, electrically conductive ink by 65-80% polymerizable organosilicon monomer, 19-34% electro-conductive material and 0.1-1% catalyzer is jointly composite forms.
3. according to the organosilicon electrically conductive ink of the wash resistant fold resistant described in claim 1 or 2, it is characterized in that: the preparation feedback 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 reacts 2-20 hour with vinyl-terminated silicone fluid III at 80-150 DEG C in the presence of a catalyst, generates 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 add-on of catalyzer is the 0.01-5% of electrically conductive ink weight; Catalyzer is the aqueous isopropanol of Platinic chloride.
4. according to the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 3, it is characterized in that: the preparation of described end-vinyl block silicone oil II is that hydrogeneous phenyl silicone oil IV reacts 3-12 hour with vinyl-terminated silicone fluid III at 100-130 DEG C in the presence of a catalyst, 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 add-on of catalyzer is the 0.1-1% of electrically conductive ink weight.
5. by the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 1, it is characterized in that: in described end-vinyl block silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of active hydrogen is 1:1-20.
6. by the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 5, it is characterized in that: in described end-vinyl block silicone oil II medium vinyl and containing hydrogen silicone oil I, the mol ratio of active hydrogen is 1:1-5.
7., by the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 1, it is characterized in that: in described electro-conductive material, the weight ratio of graphitized carbon black and Graphite Powder 99 is 1:1-10.
8., by the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 7, it is characterized in that: in described electro-conductive material, the weight ratio of graphitized carbon black and Graphite Powder 99 is 1:1-7.
9., by the organosilicon electrically conductive ink of wash resistant fold resistant according to claim 1, it is characterized in that: described Graphite Powder 99 is the high-purity graphite powder of purity >=99.85%, its mean particle size≤30 μm.
10. by the application of organosilicon electrically conductive ink of wash resistant fold resistant according to claim 1, it is characterized in that: the organosilicon electrically conductive ink of described wash resistant fold resistant is applied in the antistatic or conducting channel of textiles.
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Citations (4)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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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