CN111254716B - Organic silicon synthetic leather with electric responsiveness and manufacturing method thereof - Google Patents
Organic silicon synthetic leather with electric responsiveness and manufacturing method thereof Download PDFInfo
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- CN111254716B CN111254716B CN202010055232.2A CN202010055232A CN111254716B CN 111254716 B CN111254716 B CN 111254716B CN 202010055232 A CN202010055232 A CN 202010055232A CN 111254716 B CN111254716 B CN 111254716B
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0009—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using knitted fabrics
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0036—Polyester fibres
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0095—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by inversion technique; by transfer processes
- D06N3/0097—Release surface, e.g. separation sheets; Silicone papers
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/047—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with fluoropolymers
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- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/02—Synthetic macromolecular fibres
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Abstract
The invention relates to organic silicon synthetic leather with electric responsiveness and a manufacturing method thereof, belonging to the technical field of manufacturing of organic silicon synthetic leather. The organic silicon synthetic leather selects the conductive carbon black to be matched with the ionic conductive agent for use, has lower volume resistivity, and the volume resistivity is less than 105Omega m, the conductivity is lasting and effective; the conductive surface glue layer, the conductive bottom glue layer and the base material layer are sequentially stacked, so that the conductive adhesive tape has good performances of scraping resistance, wear resistance and the like; meanwhile, the production process of the invention is simple.
Description
Technical Field
The invention relates to organic silicon synthetic leather with electric responsiveness and a manufacturing method thereof, belonging to the technical field of manufacturing of organic silicon synthetic leather.
Background
The organic silicon synthetic leather as a new synthetic leather product for the current hot door has the characteristics of natural hydrolysis resistance, antifouling property, weather resistance and the like. Particularly, the solvent-free manufacturing technology is adopted, so that the phenomenon of large amount of organic solvents such as DMF, MEK and the like and plasticizers in polyurethane synthetic leather and PVC artificial leather is avoided, and the attention degree in recent years is higher. However, despite its significant advantages over conventional leather materials, it also has some significant disadvantages, for example, silicone materials have a very high bulk resistance, typically 1016Omega m, belonging to the insulating material. Therefore, the surface material used as synthetic leather has the defects of high surface resistance, large static electricity, easy dust absorption and the like.
Generally, in order to reduce the resistance value, metal powder, conductive carbon black, antistatic agent, etc. are added to the silicone material to increase the conductivity of the bulk material. However, the materials such as metal powder, conductive carbon black and other conductive powders are generally filled in a relatively large amount, which seriously affects the mechanical properties of the materials, so that the scratch resistance and wear resistance of the surface of the formed organosilicon synthetic leather are poor. Although the addition amount of the antistatic agent is relatively small, the action mechanism of the antistatic agent is that a layer of water film is formed on the surface of the material by absorbing moisture in the air, the range of reducing the resistance value is very limited, and the resistance value can only be generally 109-1010Omega m or so. For some applications where high electrical conductivity is desired, for example where the surface is desired to have an electrical response (typically a resistance value of less than 10 is required5Ω × m) then it appears to be stranded.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the organic silicon synthetic leather with electric responsiveness and the manufacturing method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the organic silicon synthetic leather with the electric responsiveness is composed of three layers of materials, namely a conductive surface glue layer, a conductive bottom glue layer and a base material layer from top to bottom;
the preparation raw materials of the conductive surface glue layer comprise the following components in parts by weight: 100 parts of base adhesive, 10-60 parts of vinyl silicone resin, 5-30 parts of vinyl silicone oil, 1-20 parts of hydrogen-containing silicone oil, 10-30 parts of polytetrafluoroethylene microspheres, 3-20 parts of ionic conductive agent, 0.1-5 parts of platinum catalyst and 0.01-3 parts of inhibitor;
the preparation raw materials of the conductive primer layer comprise the following components in parts by weight: 100 parts of base rubber, 5-40 parts of vinyl silicone resin, 5-20 parts of methyl silicone resin, 10-30 parts of vinyl silicone oil, 1-20 parts of hydrogen-containing silicone oil, 3-20 parts of ionic conductive agent, 0.1-5 parts of platinum catalyst and 0.01-3 parts of inhibitor;
the base material layer is one of terylene, aramid fiber, acrylic fiber, chinlon, vinylon, viscose fiber, spandex, glass fiber and pre-oxidized fiber or the blended spinning of the materials;
the base rubber comprises the following components in parts by weight: 100 parts of vinyl silicone oil, 10-40 parts of white carbon black, 20-50 parts of conductive carbon black, 5-15 parts of silazane, 1-3 parts of vinyl trimethoxy silane and 1-10 parts of water.
As a preferred embodiment of the organic silicon synthetic leather, in the conductive surface glue layer, the dosage of the ionic conductive agent is 10-15 parts, and the dosage of the vinyl silicone resin is 20-40 parts; in the conductive bottom glue layer, the dosage of the ionic conductive agent is 10-15 parts.
As a preferable embodiment of the organic silicon synthetic leather, the thickness of the conductive surface glue layer is 10-200 μm, and the thickness of the conductive bottom glue layer is 10-1000 μm.
As a preferred embodiment of the silicone synthetic leather of the present invention, a molar ratio of the active hydrogen content to the vinyl content in the conductive top glue layer is 0.5 to 5, and a molar ratio of the active hydrogen content to the vinyl content in the conductive bottom glue layer is 0.5 to 5. If the silicon-hydrogen ratio is too low, the crosslinking density is low, the mechanical strength is poor, and the wear-resisting property is not good; the silicon to hydrogen ratio is too high, dehydrogenation easily occurs, bubbles are generated, and the colloid is too brittle due to too high crosslinking density.
As a preferred embodiment of the organic silicon synthetic leather, the vinyl silicone oil is polydimethylsiloxane containing at least two vinyl groups connected with silicon atoms on a molecular chain, the vinyl groups are positioned at the tail end or side position of the molecular chain, the vinyl silicone oil can be straight chain or branched chain, or a combination thereof, the viscosity of the vinyl silicone oil is not particularly limited, and at a temperature of 25 ℃, the viscosity of the conductive surface glue layer is preferably 2000-200000mpa.s, the viscosity of the conductive bottom glue layer is preferably 5000-100000mpa.s, the viscosity is too low, the mechanical property is too low, the viscosity is too high, the processing is difficult, the vinyl content of the vinyl silicone oil is not particularly limited, the mass fraction is preferably 0.01-2%, the content of the vinyl silicone oil in the conductive surface glue layer is further preferably 0.06-0.8%, and the content of the vinyl silicone oil in the conductive bottom glue layer is further preferably 0.1-0.8%; the conductive carbon black is at least one of conductive channel black, conductive furnace carbon black, acetylene carbon black and Ketjen black; the white carbon black has a specific surface area of 50-400m2(ii) fumed silica per gram.
As a preferred embodiment of the silicone synthetic leather, the vinyl silicone resin has a structure of at least one of MT type, MQ type, MTQ type, MDQ type, and MDT type, the number average molecular weight of the vinyl silicone resin is not particularly limited, preferably 500-; the hydrogen-containing silicone oil is polydimethylsiloxane which at least contains three active hydrogen atoms directly connected with silicon atoms on a molecular chain, the active hydrogen atoms are positioned at the tail end or lateral position of the molecular chain, the content of active hydrogen of the hydrogen-containing silicone oil is not particularly limited, the mass fraction of the conductive surface glue layer is preferably 0.1-1.6%, the mass fraction of the conductive primer layer is preferably 0.2-1.2%, the viscosity of the hydrogen-containing silicone oil is not particularly limited, and the preferred viscosity is 1-1000mpa.s, and further preferably 10-200mpa.s at the temperature of 25 ℃.
As a preferred embodiment of the organic silicon synthetic leather, the particle size of the Polytetrafluoroethylene (PTFE) microspheres is 0.1-5 μm, and the PTFE microspheres are an assistant for providing smoothness and antifouling property on the surface of a coating; the ionic conductive agent is at least one of quaternary ammonium salt conductive agents, imidazole conductive agents, pyridine conductive agents, quaternary phosphonium conductive agents, pyrrolidine conductive agents, and piperidine conductive agents, and examples thereof include quaternary ammonium salt conductive agents such as tetraethylammonium, tetrabutylammonium, dodecyltrimethylammonium, hexadecyltrimethylammonium, octadecyltrimethylammonium, tributylmethylammonium bis (trifluoromethanesulfonyl) imide salt, tributylmethylammonium chloride, and N-methoxyethyl-N-methyldiethylammonium tetrafluoroborate; imidazole-based conductive agents such as 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium bromide, 1-ethyl-3-methylimidazolium iodide, and 1-ethyl-3-methylimidazolium hexafluorophosphate; pyridine conductive agents such as N-octylpyridinium bromide, N-hexylpyridinium bis (trifluoromethanesulfonyl) imide, N-hexylpyridinium hexafluorophosphate, and N-hexylpyridinium tetrafluoroborate; quaternary phosphonium-based conductive agents such as N-hexylpyridinium tetrafluoroborate, tributylhexylphosphonium bromide, tetrabutylphosphonium bis (trifluoromethanesulfonyl) imide salts, and pyrrolidine-based conductive agents such as N-butyl-N-methylpyrrolidine bis (trifluoromethanesulfonyl) imide salts and N-butyl-N-methylpyrrolidine bromide salts; and piperidine-based conductive agents such as N-butyl-N-methylpiperidine bis (trifluoromethanesulfonyl) imide salt and N-butyl-N-methylpiperidine bromide salt.
As a preferred embodiment of the silicone synthetic leather of the present invention, the platinum catalyst is platinum black, platinum-supported nano alumina powder, platinum-supported nano silica powder, chloroplatinic acid, a reactant of chloroplatinic acid and monohydric alcohol, a complex of platinum and alkenylsiloxane, or thermoplastic resin powder coated with platinum, the mass concentration of platinum in the platinum catalyst is 1%, the platinum catalyst is mainly used for promoting the crosslinking reaction of vinyl and active hydrogen reaction, the amount of platinum used in the conductive surface glue layer is 1 to 3000ppm of the total mass of the raw materials, and the amount of platinum used in the conductive primer layer is 1 to 5000ppm of the total mass of the raw materials; the inhibitor is at least one of an alkynol compound, a polyvinyl siloxane and a polysiloxane, an amide compound and a maleate compound, and examples thereof include alkynol compounds such as 3-methyl-1-butyn-3-ol, 3-methyl-1-pentyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol and 1-ethynyl-1-cyclohexanol, alkenyl silicone oils, polyvinyl siloxanes such as methylvinylcyclotetrasiloxane and the like, and polysiloxanes; amide compounds such as N, N-diallylcarboxamide and N, N, N ', N' -tetraallylphthalic amide, and maleate compounds such as monoallyl maleate.
As a preferred embodiment of the silicone synthetic leather of the present invention, the structure of the methyl silicone resin is at least one of MT type, MQ type, MTQ type, MDQ type, and MDT type, and the number average molecular weight is not particularly limited, and is preferably 2000-.
In a preferred embodiment of the silicone synthetic leather of the present invention, the structure of the substrate layer is a knitted structure, a woven structure or a non-woven structure, the substrate layer is inelastic, double-sided stretch or four-sided stretch, the substrate may be microfiber or genuine leather, and the thickness of the substrate is not limited, and is preferably 0.1 to 3.0 mm.
In a second aspect, the invention provides a preparation method of the organic silicon synthetic leather, which comprises the following steps:
(1) putting vinyl silicone oil, white carbon black, conductive carbon black, silazane, vinyl trimethoxy silane and water into a kneading machine in sequence, heating the kneading machine to 100-140 ℃ for treatment for 1h, then heating the kneading machine to 150-180 ℃ for vacuumizing for 1h, and grinding for 1 time by a three-roll machine after the temperature is recovered to room temperature to obtain the base adhesive;
(2) putting the base glue, vinyl silicone resin, vinyl silicone oil, hydrogen-containing silicone oil, polytetrafluoroethylene microspheres, an ionic conductive agent, a platinum catalyst and an inhibitor into a planetary machine in sequence, opening cooling water, vacuumizing, dispersing and stirring for 30min to obtain the conductive surface glue;
(3) sequentially putting the base adhesive, vinyl silicone resin, methyl silicone resin, vinyl silicone oil, hydrogen-containing silicone oil, an ionic conductive agent, a platinum catalyst and an inhibitor into a planetary machine, and cooling, dispersing and stirring for 30min to obtain the conductive primer;
(4) coating the conductive surface glue prepared in the step (2) on release paper, controlling the coating thickness to be 10-200 mu m, sending the release paper into a drying oven at 80-150 ℃, baking for 1-10min for curing, coating the conductive primer prepared in the step (3) on the cured conductive surface glue layer, controlling the coating thickness to be 10-1000 mu m, then attaching the base material to the conductive primer layer through a pressure roller, sending the base material into a baking oven at 80-150 ℃, baking for 2-15min for curing, and peeling the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Compared with the prior art, the invention has the beneficial effects that: the organic silicon synthetic leather selects the conductive carbon black to be matched with the ionic conductive agent for use, has lower volume resistivity, and the volume resistivity is less than 105Omega m, the conductivity is lasting and effective; the conductive surface adhesive layer, the conductive bottom adhesive layer and the base material layer are sequentially superposed, so that the conductive adhesive tape has better performances of scraping resistance, wear resistance and the like; meanwhile, the production process of the invention is simple.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinylSilicone oil, 25 parts of specific surface area 150m2Putting the silica white, 30 parts of acetylene black, 10 parts of silazane, 3 parts of vinyl trimethoxy silane and 3 parts of water into a kneader in sequence, heating the kneader to 130 ℃ for treatment for 1h, then heating the kneader to 160 ℃ and vacuumizing for 1h, and grinding for 1 time on a three-roll machine after the temperature is restored to room temperature to obtain the base adhesive;
(2) 100 parts of the base glue, 30 parts of vinyl silicone resin (MT type, number average molecular weight: 10000, Vi: 1.3%), 10 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 6 parts of hydrogen-containing silicone oil (viscosity: 200mpa.s, H: 0.8%), 20 parts of PTFE microspheres (particle size: 3 mu m), 8 parts of tetrabutylammonium, 1 part of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.5 part of 3-methyl-1-butyn-3-ol are put into a planetary machine in sequence, cooling water is opened, and the mixture is dispersed and stirred for 30min in vacuum, so that the conductive face glue is obtained;
(3) 100 parts of the base adhesive, 20 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 15 parts of methyl silicone resin (MQ type, number average molecular weight: 3000), 15 parts of vinyl silicone oil (viscosity: 3000mpa.s, Vi: 0.14%), 10 parts of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 0.50%), 8 parts of 1-ethyl-3-methylimidazolium bromide, 2 parts of platinic acid catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), and 0.8 part of 3-methyl-1-butyn-3-ol are put into a planetary machine in sequence, and cooled, stirred and dispersed for 30min to obtain the conductive base adhesive;
(4) coating the conductive surface glue on release paper, coating the conductive surface glue to the thickness of 100 mu m, sending the release paper into a drying oven at 100 ℃, baking for 5min for curing, coating the conductive primer on the cured conductive surface glue layer to the thickness of 100 mu m, then attaching the double-sided elastic polyester knitted base fabric with the thickness of 0.5mm to the conductive primer layer through a pressure roller, sending the conductive primer into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Example 2
An organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinyl silicone oil and 35 parts ofArea of 150m2Putting the silica white, 20 parts of acetylene black, 10 parts of silazane, 3 parts of vinyl trimethoxy silane and 3 parts of water into a kneader in sequence, heating the kneader to 130 ℃ for treatment for 1h, then heating the kneader to 160 ℃ and vacuumizing for 1h, and grinding for 1 time on a three-roll machine after the temperature is restored to room temperature to obtain the base adhesive;
(2) putting 100 parts of the base glue, 25 parts of vinyl silicone resin (MTQ type, the number average molecular weight: 5000, Vi: 2.8%), 10 parts of vinyl silicone oil (the viscosity: 10000mpa.s, Vi: 0.14%), 6 parts of hydrogen-containing silicone oil (the viscosity: 200mpa.s, H: 1.0%), 20 parts of PTFE microspheres (the particle size: 3 mu m), 15 parts of tetrabutylammonium, 1.3 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.5 part of 3-methyl-1-butyn-3-ol into a planetary machine in sequence, opening cooling water, vacuumizing, dispersing and stirring for 30min to obtain the conductive surface glue;
(3) 100 parts of the base adhesive, 25 parts of vinyl silicone resin (MTQ type, number average molecular weight: 15000, Vi: 1.6%), 15 parts of methyl silicone resin (MQ type, number average molecular weight: 3000%), 15 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 10 parts of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 1.0%), 20 parts of N-hexylpyridine tetrafluoroborate, 2 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.8 part of 3-methyl-1-butyn-3-ol are put into a planetary machine in sequence, and cooled, dispersed and stirred for 30min to obtain the conductive primer;
(4) coating the conductive surface glue on release paper, coating the conductive surface glue to the thickness of 100 micrometers, sending the release paper into a drying oven at 100 ℃, baking for 5min for curing, coating the conductive primer on the cured conductive surface glue layer to the thickness of 100 micrometers, then attaching the inelastic polyester woven base fabric with the thickness of 1.0mm to the conductive primer layer through a pressure roller, sending the conductive base fabric into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Example 3
An organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinyl silicone oil and 15 parts of specific surface areaIs 150m2Putting the silica white, 40 parts of acetylene black, 12 parts of silazane, 2 parts of vinyl trimethoxy silane and 3 parts of water into a kneader in sequence, heating the kneader to 130 ℃ for treatment for 1h, then heating the kneader to 160 ℃ and vacuumizing for 1h, and grinding for 1 time on a three-roll machine after the temperature is restored to room temperature to obtain the base adhesive;
(2) 100 parts of the base glue, 15 parts of vinyl silicone resin (MTQ type, number average molecular weight: 5000, Vi: 2.8%), 25 parts of vinyl silicone oil (viscosity: 20000mpa.s, Vi: 0.2%), 6 parts of hydrogen-containing silicone oil (viscosity: 200mpa.s, H: 1.0%), 20 parts of PTFE microspheres (particle size: 3 μm), 15 parts of tetrabutylammonium, 1.3 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.5 part of 3-methyl-1-butyn-3-ol are sequentially put into a planetary machine, cooling water is turned on, and vacuum pumping is carried out for dispersion stirring for 30min to obtain the conductive surface glue;
(3) putting 100 parts of the base adhesive, 25 parts of vinyl silicone resin (MTQ type, number average molecular weight: 15000, Vi: 1.6%), 15 parts of methyl silicone resin (MQ, number average molecular weight: 3000), 15 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 10 parts of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 1.0%), 20 parts of N-hexyl pyridine tetrafluoroborate, 2 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.8 part of 3-methyl-1-butyn-3-ol into a planetary machine in sequence, cooling, dispersing in water, and stirring for 30min to obtain the conductive primer;
(4) coating the conductive surface glue on release paper, coating the conductive surface glue to the thickness of 100 micrometers, sending the release paper into a drying oven at 100 ℃, baking for 5min for curing, coating the conductive primer on the cured conductive surface glue layer to the thickness of 100 micrometers, then attaching inelastic polyester woven base cloth with the thickness of 1.0mm to the conductive primer layer through a pressure roller, sending the conductive primer layer into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Example 4
The organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinyl silicone oil and 15 parts of vinyl silicone oil with the specific surface area of 150m2Putting the white carbon black, 40 parts of acetylene black, 12 parts of silazane, 2 parts of vinyl trimethoxy silane and 3 parts of water into a kneader in sequence, heating the kneader to 130 ℃ for processing for 1h, then heating the kneader to 160 ℃ and vacuumizing for 1h, and grinding for 1 time on a three-roller machine after the temperature is recovered to room temperature to obtain the base adhesive;
(2) 100 parts of the base glue, 35 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 25 parts of vinyl silicone oil (viscosity: 20000mpa.s, Vi: 0.2%), 4 parts of hydrogen-containing silicone oil (viscosity: 200mpa.s, H: 1.5%), 25 parts of PTFE microspheres (particle size: 1 μm), 15 parts of tetrabutylammonium, 1.3 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.6 part of N, N-diallylformamide are put into a planetary machine in sequence, cooling water is opened, and the mixture is dispersed and stirred for 30min in a vacuum pumping manner to obtain the conductive dough glue;
(3) 100 parts of the base adhesive, 15 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 20 parts of methyl silicone resin (MQ type, number average molecular weight: 5000), 15 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 10 parts of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 1.0%), 10 parts of N-hexyl pyridine tetrafluoroborate, 2 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.6 part of N, N-diallyl formamide are sequentially added into a planetary machine, and cooling, water dispersion and stirring are carried out for 30min to obtain the conductive primer;
(4) coating the conductive surface glue on release paper, coating the conductive surface glue to the thickness of 100 mu m, sending the release paper into a drying oven at 120 ℃, baking for 4min for curing, coating the conductive primer on the cured conductive surface glue layer to the thickness of 100 mu m, then attaching the microfiber with the thickness of 1.0mm onto the conductive primer layer through a pressure roller, sending the conductive primer into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Example 5
An organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinyl silicone oil and 10 parts of silicone oil with a specific surface area of 150m2White carbon black per gram, 50 portionsPutting acetylene black, 5 parts of silazane, 3 parts of vinyltrimethoxysilane and 1 part of water into a kneading machine in sequence, heating the kneading machine to 130 ℃ for treatment for 1h, then heating the kneading machine to 160 ℃ for vacuumizing for 1h, and grinding for 1 time by a three-roll machine after the temperature is restored to room temperature to obtain the base adhesive;
(2) 100 parts of the base glue, 10 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 5 parts of vinyl silicone oil (viscosity: 20000mpa.s, Vi: 0.2%), 20 parts of hydrogen-containing silicone oil (viscosity: 200mpa.s, H: 1.5%), 10 parts of PTFE microspheres (particle size: 1 μm), 3 parts of tetrabutylammonium, 0.1 part of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.01 part of N, N-diallylformamide are sequentially put into a planetary machine, cooling water is turned on, and the mixture is dispersed and stirred for 30min in a vacuum pumping manner to obtain the conductive surface glue;
(3) 100 parts of the base adhesive, 5 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 20 parts of methyl silicone resin (MQ type, number average molecular weight: 5000), 10 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 1 part of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 1.0%), 20 parts of N-hexyl pyridine tetrafluoroborate, 0.1 part of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 0.01 part of N, N-diallyl formamide are sequentially added into a planetary machine, and cooling, water dispersion and stirring are carried out for 30min to obtain the conductive primer;
(4) coating the conductive surface glue on release paper, coating the conductive surface glue with the thickness of 10 mu m, sending the release paper into a drying oven at 120 ℃, baking for 4min for curing, coating the conductive primer on the cured conductive surface glue layer with the thickness of 10 mu m, then attaching the microfiber with the thickness of 1.0mm onto the conductive primer layer through a pressure roller, sending the conductive primer into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Example 6
An organic silicon synthetic leather with electric responsiveness is prepared by the following preparation method:
(1) 100 parts of vinyl silicone oil and 40 parts of silicone oil with the specific surface area of 150m2White carbon black per gram, 20 parts of acetylene black, 15 parts of silazane,Putting 1 part of vinyltrimethoxysilane and 10 parts of water into a kneader in sequence, heating the kneader to 130 ℃ for treatment for 1h, then heating the kneader to 160 ℃, vacuumizing for 1h, and grinding for 1 time by a three-roll machine after the temperature is recovered to room temperature to obtain base glue;
(2) 100 parts of the base adhesive, 60 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 30 parts of vinyl silicone oil (viscosity: 20000mpa.s, Vi: 0.2%), 1 part of hydrogen-containing silicone oil (viscosity: 200mpa.s, H: 1.5%), 30 parts of PTFE microspheres (particle size: 1 μm), 20 parts of tetrabutylammonium, 5 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), and 3 parts of N, N-diallylformamide are sequentially put into a planetary machine, cooling water is opened, and vacuum pumping is performed to disperse and stir for 30min, so that the conductive face adhesive is obtained;
(3) 100 parts of the base rubber, 40 parts of vinyl silicone resin (MT type, number average molecular weight: 8000, Vi: 1.6%), 5 parts of methyl silicone resin (MQ type, number average molecular weight: 5000), 30 parts of vinyl silicone oil (viscosity: 10000mpa.s, Vi: 0.14%), 20 parts of hydrogen-containing silicone oil (viscosity: 50mpa.s, H: 1.0%), 3 parts of N-hexyl pyridine tetrafluoroborate, 5 parts of platinum catalyst (chloroplatinic acid isopropanol solution, Pt concentration wt 1%), 3 parts of N, N-diallyl formamide are sequentially put into a planetary machine, and cooling, water dispersion and stirring are carried out for 30min to obtain the conductive primer;
(4) coating the conductive surface glue on the release paper, coating the conductive surface glue to the thickness of 200 mu m, sending the release paper into a drying oven at 120 ℃, baking for 4min for curing, coating the conductive primer on the cured conductive surface glue layer to the thickness of 1000 mu m, then attaching the microfiber with the thickness of 1.0mm onto the conductive primer layer through a pressure roller, sending the conductive primer into the drying oven at 140 ℃, baking for 3min for curing, and stripping the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
Effect example 1
For the above examples 1 to 6, the wear resistance, scratch resistance and conductivity were evaluated by the following methods, and the test results are shown in table 1.
Wear resistance:
the test was carried out according to ISO/NP17076-2004, using a CS-10 grinding wheel, a load of 1000g and a test revolution of 3000 revolutions. And (4) judging the standard: grade 1- -very obvious, grade 2- -more obvious, grade 3- -distinguishable, grade 4- -indistinguishable, grade 5- -indistinguishable.
The test was carried out as specified in ASTM D4157-13, using a No. 10 canvas cotton, with a test period of 300000 cycles. And (4) judging the standard: level 1- -the coating is abraded through, revealing the base fabric; level 2- -the coating is abraded more seriously, the lines are ground flat; grade 3- -the coating lines are worn, but the lines can be seen clearly; grade 4- -there is almost no wear on the coating lines, but there is slight variation in haze; grade 5- -no trace of abrasion was seen with the coating, and the haze was unchanged.
Scratch resistance:
a long-gauge paper clip with a size of about 32mm by 7mm was used to apply a force of 7.5N to the surface of the sample, and the surface of the leather was repeatedly scratched for 200 cycles, and then observed with a microscope of 10 times for the presence or absence of any phenomena such as breakage, and falling off.
And (3) resistance testing:
the test was carried out according to the "four-point probe array" technique specified in JIS K7194.
TABLE 1
As can be seen from table 1, examples 1-6 have significant properties of abrasion resistance, scratch resistance, and lower volume resistivity, thus evidencing the rationality and practical effectiveness of the proposed solution.
Effect example 2
In the invention, the performance of the organic silicon synthetic leather is influenced by the dosage of the ionic conductive agent in the conductive surface glue layer, the dosage of the vinyl silicone resin and the dosage of the ionic conductive agent in the conductive primer layer. Test groups 1-5 are set to examine the influence of the dosage of the ionic conductive agent and the dosage of the vinyl silicone resin on the performance of the organic silicon synthetic leather. In test groups 1-5, only the amount of the ionic conductive agent in the conductive surface adhesive layer, the amount of the vinyl silicone resin and the amount of the ionic conductive agent in the conductive primer layer are different, and the other components and the preparation method are the same. The amount of the ionic conductive agent in the conductive primer layer, the amount of the vinyl silicone resin in the conductive primer layer, and the amount of the ionic conductive agent in the conductive primer layer are shown in table 2. Meanwhile, the performance of the test groups 1 to 5 was tested, and the test results are shown in table 3.
TABLE 2
TABLE 3
As can be seen from Table 3, the amount of the ionic conductive agent in the conductive surface glue layer, the amount of the vinyl silicone resin in the conductive primer layer and the amount of the ionic conductive agent in the conductive primer layer affect the performance of the organic silicon synthetic leather of the present invention. When the dosage of the ionic conductive agent in the conductive surface glue layer is 10-15 parts, the dosage of the vinyl silicone resin is 20-40 parts, and the dosage of the ionic conductive agent in the conductive bottom glue layer is 10-15 parts, the comprehensive performance of the prepared organic silicon synthetic leather is optimal.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The organic silicon synthetic leather with the electric responsiveness is characterized by comprising three layers of materials, namely a conductive surface glue layer, a conductive bottom glue layer and a base material layer from top to bottom;
the preparation raw materials of the conductive surface glue layer comprise the following components in parts by weight: 100 parts of base adhesive, 10-60 parts of vinyl silicone resin, 5-30 parts of vinyl silicone oil, 1-20 parts of hydrogen-containing silicone oil, 10-30 parts of polytetrafluoroethylene microspheres, 3-20 parts of ionic conductive agent, 0.1-5 parts of platinum catalyst and 0.01-3 parts of inhibitor;
the preparation raw materials of the conductive primer layer comprise the following components in parts by weight: 100 parts of base rubber, 5-40 parts of vinyl silicone resin, 5-20 parts of methyl silicone resin, 10-30 parts of vinyl silicone oil, 1-20 parts of hydrogen-containing silicone oil, 3-20 parts of ionic conductive agent, 0.1-5 parts of platinum catalyst and 0.01-3 parts of inhibitor;
the base material layer is one of terylene, aramid fiber, acrylic fiber, chinlon, vinylon, viscose fiber, spandex, glass fiber and pre-oxidized fiber or the blended spinning of the materials;
the base rubber comprises the following components in parts by weight: 100 parts of vinyl silicone oil, 10-40 parts of white carbon black, 20-50 parts of conductive carbon black, 5-15 parts of silazane, 1-3 parts of vinyl trimethoxy silane and 1-10 parts of water;
the vinyl silicon resin has at least one of MT type, MQ type, MTQ type, MDQ type and MDT type;
the molar ratio of the active hydrogen content to the vinyl content in the conductive surface glue layer is 0.5-5, and the molar ratio of the active hydrogen content to the vinyl content in the conductive bottom glue layer is 0.5-5;
the mass fraction of vinyl in the vinyl silicone resin is 0.1-5%, and the mass fraction of vinyl in the vinyl silicone oil is 0.01-2%;
the particle size of the polytetrafluoroethylene microsphere is 0.1-5 μm;
the conductive carbon black is at least one of conductive channel black, conductive furnace carbon black, acetylene carbon black and Ketjen black;
the ionic conductive agent is at least one of quaternary ammonium salt conductive agent, imidazole conductive agent, pyridine conductive agent, quaternary phosphonium conductive agent, pyrrolidine conductive agent and piperidine conductive agent.
2. The silicone synthetic leather according to claim 1, wherein in the conductive surface glue layer, the amount of the ionic conductive agent is 10 to 15 parts, and the amount of the vinyl silicone resin is 20 to 40 parts; in the conductive bottom glue layer, the dosage of the ionic conductive agent is 10-15 parts.
3. The silicone synthetic leather of claim 1, wherein the thickness of the conductive top coat layer is 10-200 μ ι η and the thickness of the conductive primer layer is 10-1000 μ ι η.
4. The silicone synthetic leather of claim 1, wherein the vinyl silicone oil is polydimethylsiloxane having at least two vinyl groups attached to silicon atoms in a molecular chain, the vinyl groups being located at the terminal or lateral position of the molecular chain; the white carbon black has a specific surface area of 50-400m2(ii) fumed silica per gram.
5. The silicone synthetic leather of claim 1, wherein the hydrogen-containing silicone oil is polydimethylsiloxane having at least three active hydrogen atoms directly bonded to silicon atoms on a molecular chain, the active hydrogen atoms being at the terminal or lateral positions of the molecular chain.
6. The silicone synthetic leather according to claim 1, wherein the platinum catalyst is platinum black, platinum-supported nano alumina powder, platinum-supported nano silica powder, chloroplatinic acid, a reactant of chloroplatinic acid and monohydric alcohol, a complex of platinum and alkenylsiloxane, or thermoplastic resin powder internally coated with platinum, and the mass concentration of platinum in the platinum catalyst is 1%; the inhibitor is at least one of alkynol compound alkenyl silicone oil, polyvinyl siloxane and polysiloxane, amide compound and maleate compound.
7. The silicone synthetic leather according to claim 1, wherein the methyl silicone resin has a structure of at least one of MT type, MQ type, MTQ type, MDQ type, and MDT type.
8. The silicone synthetic leather of claim 1, wherein the structure of the substrate layer is a knitted structure, a woven structure, or a non-woven structure, and the substrate layer is inelastic, double-sided, or four-sided.
9. The method for preparing the silicone synthetic leather according to any one of claims 1 to 8, comprising the steps of:
(1) putting vinyl silicone oil, white carbon black, conductive carbon black, silazane, vinyl trimethoxy silane and water into a kneading machine in sequence, heating the kneading machine to 100-140 ℃ for treatment for 1h, then heating the kneading machine to 150-180 ℃ for vacuumizing for 1h, and grinding for 1 time by a three-roll machine after the temperature is recovered to room temperature to obtain the base adhesive;
(2) putting the base glue, vinyl silicone resin, vinyl silicone oil, hydrogen-containing silicone oil, polytetrafluoroethylene microspheres, an ionic conductive agent, a platinum catalyst and an inhibitor into a planetary machine in sequence, opening cooling water, vacuumizing, dispersing and stirring for 30min to obtain the conductive surface glue;
(3) sequentially putting the base adhesive, vinyl silicone resin, methyl silicone resin, vinyl silicone oil, hydrogen-containing silicone oil, an ionic conductive agent, a platinum catalyst and an inhibitor into a planetary machine, and cooling, dispersing and stirring for 30min to obtain the conductive primer;
(4) coating the conductive surface glue prepared in the step (2) on release paper, controlling the coating thickness to be 10-200 mu m, sending the release paper into a drying oven at 80-150 ℃, baking for 1-10min for curing, coating the conductive primer prepared in the step (3) on the cured conductive surface glue layer, controlling the coating thickness to be 10-1000 mu m, then attaching a base material to the conductive primer layer through a pressure roller, sending the conductive primer layer into a drying oven at 80-150 ℃, baking for 2-15min for curing, and peeling the release paper from the cured synthetic leather to obtain the organic silicon synthetic leather with electric responsiveness.
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