CN103173018A - Flame-retardant liquid silicon rubber for coating fiber materials and preparation method of rubber - Google Patents
Flame-retardant liquid silicon rubber for coating fiber materials and preparation method of rubber Download PDFInfo
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Abstract
The invention discloses flame-retardant liquid silicon rubber for coating fiber materials and a preparation method of the rubber. The liquid silicon rubber is composed of an ingredient A and an ingredient B according to a mass ratio of 1:10 to 10:1, wherein the ingredient A is composed of base rubber, a platinum complex and a tackifier according to certain proportion, the ingredient B is composed of base rubber, hydrogen polysiloxane, an alkynol inhibitor and a tackifier according to certain proportion, and the base rubber is composed of three vinyl-terminated organopolysiloxane with different viscosities and vinyl content, silicon dioxide and a fire retardant according to certain proportion. The preparation method of the liquid silicon rubber comprises the steps of preparing the base rubber, the ingredient A and the ingredient B sequentially, and uniformly mixing the ingredient A with the ingredient B according to a mass ratio. The liquid silicon rubber disclosed by the invention has the advantages of temperature resistance, corrosion resistance, insulation, non-toxicity, environmental friendliness, low energy consumption and the like, can be directly coated on various fiber cloth, has a wide range of application, is low in cost and has an industrial application value. The preparation method of the liquid silicon rubber is simple and practicable.
Description
Technical field
The present invention relates to a kind of liquid silastic and preparation method thereof, specifically, relate to a kind of filamentary material coating with anti-flaming liquid silicon rubber and preparation method thereof, belong to the silastic material technical field.
Background technology
Weaving fiber cloth or non woven fibre cloth comprise: glasscloth, Silon cloth, acetate fibre cloth, nonwoven polyester cloth etc., silicon rubber is one of its coating material.The cloth goods of these coating silicon rubbers have good use properties, for example: heatproof, resistance to chemical attack, breaking tenacity, tear strength are high, now have been widely used in the fields such as building, the connection of electric insulation pipeline flexible, chemical anticorrosion and sealing.The silicon rubber molecule is to form major key with-Si-O-key, and this bond dissociation energy is very big.Traditional silicone rubber coating is that the solid rubber unvulcanizate is formulated with the non-polar solvent dissolving.These non-polar solvent great majority are poisonous, inflammable substance, and such as gasoline, toluene, dimethylbenzene, vinyl acetate etc., contaminate environment not only, affect the healthy of operating worker, but also have dangerous production hidden danger in actual use.
Summary of the invention
In view of the foregoing defects the prior art has, the purpose of this invention is to provide a kind of filamentary material coating with good flame retardant resistance, cementability and environmental-protecting performance with anti-flaming liquid silicon rubber and preparation method thereof, with the widespread use requirement of the cloth goods that satisfy coating silicon rubber.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of filamentary material coating anti-flaming liquid silicon rubber is to form in 1: 10～10: 1 by A component and B component in mass ratio; Wherein,
The compositing formula of A component is as follows:
Base glue 100 mass parts
Platinum complex compound 0.2～1.0 mass parts
Tackifier 0.2～5.0 mass parts;
The compositing formula of B component is as follows:
The compositing formula of described basic glue is as follows:
Above-mentioned per-cent is mass percent, and the mass percent sum of described composition is 100%; Described polysiloxane I is that the viscosity 25 ℃ of mensuration is that 5000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.25～0.5wt.%; Described polysiloxane II is that the viscosity 25 ℃ of mensuration is that 1500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.0wt.%; Described polysiloxane III is that the viscosity 25 ℃ of mensuration is that 250～1500cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 1～10wt.%; The composition general formula of the organopolysiloxane of described ethenyl blocking is: R
2SiO (SiRR ' O)
nSiR
2, R wherein is vinyl, R ' is vinyl or methyl.
A kind of described filamentary material coating comprises the steps: with the preparation method of anti-flaming liquid silicon rubber
A) prepare basic glue
1. the polysiloxane I of 80～100% formula ratios and polysiloxane II, silicon-dioxide and the fire retardant of formula ratio are added in kneader, at room temperature mediated 1～2 hour;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1～2 hour;
3. vacuumize, continue to mediate 2～4 hours in 150～160 ℃ under vacuum condition, then stop vacuumizing, be cooled to 110～130 ℃, add the polysiloxane I of remaining formula ratio and the polysiloxane III of formula ratio, mix, namely get described basic glue;
B) preparation A component
Get basic glue 100 mass parts, then add platinum complex compound and the tackifier of formula ratio, mix, namely get described A component;
C) preparation B component
Get basic glue 100 mass parts, then add hydrogen containing siloxane, alkynol class inhibitor and the tackifier of formula ratio, mix, namely get described B component;
D) be to mix in 1: 10～10: 1 in mass ratio with the A component that makes and B component, namely get described filamentary material coating anti-flaming liquid silicon rubber.
As further preferred version, described platinum complex compound is to be formed by Platinic chloride and divinyl dimethyl sily oxide, and platinum content wherein is 1000～5000ppm.
As further preferred version, described tackifier are selected from any one or the mixture more than two kinds in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-aminopropyl triethoxysilane.
As further preferred version, the hydrogen content in described hydrogen containing siloxane is 0.2～1.2wt.%, and the polymerization degree is 20～50.
As further preferred version, described alkynol class inhibitor is to be to mix in 1: 1～5: 1 in mass ratio by ethynyl-1-hexalin and 2-methyl-3-butyne-2-alcohol.
As further preferred version, described silicon-dioxide is aerosil or the precipitated silica after silane coupling agent is done the hydrophobic processing.
As further preferred version, described fire retardant is made hydrophobic through silane coupling agent and is processed.
As further preferred version, described fire retardant is selected from any one or the mixture more than two kinds in aluminium hydroxide, antimonous oxide, TDE, decabromodiphynly oxide, mica powder.
As preferred version further, describedly make hydrophobic through silane coupling agent and process, refer to object being treated and silane coupling agent be in mass ratio mixed in 5: 1～10: 1 after, 120～130 ℃ of stirring reactions 5～7 hours; Described silane coupling agent is selected from any one or the mixture more than two kinds in hexamethyldisilazane, dimethyldiethoxysilane, dimethyldimethoxysil,ne, dimethyldichlorosilane(DMCS), dimethyl cyclosiloxane.
liquid silastic provided by the invention has splendid mobility, flame retardant resistance and stronger cementability, need not add still what organic solvent, can directly be applied on various cloth, then heated 5～10 minutes in not higher than the drying tunnel of 150 ℃, can obtain being rich in gloss, the cloth goods of the coating silicon rubber that feel is superior, described cloth goods Applicable temperature wide (70～230 ℃), weathering resistance is good, anti-ozone, light and weathering age, (specific inductivity is 3～3.2 to have high insulating property, voltage breakdown is 20～50KV/mm), flexible, skin friction force is large, good springiness, resistance to chemical attack, do not contain various objectionable impuritiess, meet the U.S. and European food test standard, can satisfy electrical apparatus insulation, non-metal compensator, anticorrosion, heatproof, the building sealing, the material application requiring in the fields such as high-temperature anticorrosion.
Therefore; compared with prior art; a kind of filamentary material coating provided by the invention has significance progress and beneficial effect with anti-flaming liquid silicon rubber; have heatproof, corrosion resistant, insulation, the plurality of advantages such as nontoxic; applied widely, and its preparation method is simple, and with low cost; be fit to large-scale production, have industrial applications and be worth.
Embodiment
Below in conjunction with embodiment, the present invention is done further detailed, complete explanation.
Embodiment 1
A) prepare basic glue
1. adding 400kg viscosity in the 1000L kneader is that 10000cp (25 ℃), contents of ethylene are the polysiloxane I of 0.45wt.%, 370kg viscosity is that 4000cp (25 ℃), contents of ethylene are the polysiloxane II of 0.68wt.%, silicon-dioxide and the 250kg fire retardant through silane coupling agent do hydrophobic processing after of 240kg after silane coupling agent is done the hydrophobic processing mediated agglomerating follow-up continuous at room temperature the kneading 2 hours;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1 hour;
3. being evacuated to vacuum tightness is 0.8MPa, continue to mediate 2 hours in 150～160 ℃ under vacuum condition, then stop vacuumizing, be cooled to 120 ℃, adding 50kg viscosity is that 10000cp (25 ℃), contents of ethylene are that polysiloxane I and the 20kg viscosity of 0.45wt.% is that 500cp (25 ℃), contents of ethylene are the polysiloxane III of 2.5wt.%, mix, namely get described basic glue;
B) preparation A component
Get basic glue 100kg, then add 250g platinum complex compound and 1.5kg tackifier, mix, namely get described A component;
C) preparation B component
Get basic glue 100kg, then add 800g hydrogen containing siloxane, 30g alkynol class inhibitor and 1.5kg tackifier, mix, namely get described B component;
D) A component and the B component that makes mixed, namely get described filamentary material coating anti-flaming liquid silicon rubber.
The aforesaid liquid silicon rubber that makes directly is applied on glasscloth, and through 150 ℃ of bakings 5 minutes, namely obtaining thickness was that 0.01～1.5mm, coated adhesive are firm, soft, flame retardant resistance is V
0The glass complex fabric cloth of level, rich glossiness coating silicon rubber.
Embodiment 2
A) prepare basic glue
1. adding 400kg viscosity in the 1000L kneader is that 10000cp (25 ℃), contents of ethylene are the polysiloxane I of 0.45wt.%, 350kg viscosity is that 4000cp (25 ℃), contents of ethylene are the polysiloxane II of 0.68wt.%, silicon-dioxide and the 250kg fire retardant through silane coupling agent do hydrophobic processing after of 240kg after silane coupling agent is done the hydrophobic processing mediated agglomerating follow-up continuous at room temperature the kneading 1 hour;
2. be warming up to 150～160 ℃, then constant temperature was mediated 2 hours;
3. being evacuated to vacuum tightness is 0.8MPa, continue to mediate 4 hours in 150～160 ℃ under vacuum condition, then stop vacuumizing, be cooled to 120 ℃, adding 90kg viscosity is that 500cp (25 ℃), contents of ethylene are the polysiloxane III of 2.5wt.%, mix, namely get described basic glue;
B) preparation A component
Get basic glue 100kg, then add 500g platinum complex compound and 2.5kg tackifier, mix, namely get described A component;
C) preparation B component
Get basic glue 100kg, then add 2kg hydrogen containing siloxane, 100g alkynol class inhibitor and 2.5kg tackifier, mix, namely get described B component;
D) A component and the B component that makes mixed, namely get described filamentary material coating anti-flaming liquid silicon rubber.
The aforesaid liquid silicon rubber that makes directly is applied on Silon cloth, and through 150 ℃ of bakings 5 minutes, namely obtaining thickness was that 0.01～1.5mm, coated adhesive are firm, soft, flame retardant resistance is V
0The polyamine complex fabric cloth of level, rich glossiness coating silicon rubber.
Use silane coupling agent to do the operation that hydrophobic processes to silicon-dioxide as follows: silicon-dioxide is added in reaction vessel with agitating function, heat up and simultaneously silane coupling agent is sprayed in reaction vessel, be warmed up to 120～130 ℃, insulated and stirred reaction 5～7, then vacuum is deviate from by product; The mass ratio of silicon-dioxide and silane coupling agent is 5: 1～10: 1.
Use silane coupling agent to do the operation that hydrophobic processes to fire retardant as follows: fire retardant is added in reaction vessel with agitating function, heat up and simultaneously silane coupling agent is sprayed in reaction vessel, be warmed up to 120～130 ℃, insulated and stirred reaction 5～7, then vacuum is deviate from by product; The mass ratio of fire retardant and silane coupling agent is 5: 1～10: 1.
Described silane coupling agent is selected from any one or the mixture more than two kinds in hexamethyldisilazane, dimethyldiethoxysilane, dimethyldimethoxysil,ne, dimethyldichlorosilane(DMCS), dimethyl cyclosiloxane.
Platinum complex compound described in embodiment is preferably by Platinic chloride and divinyl dimethyl sily oxide and forms, and platinum content wherein is 1000～5000ppm.
Tackifier described in embodiment are preferably any one or the mixture more than two kinds in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-aminopropyl triethoxysilane.
Hydrogen content in hydrogen containing siloxane described in embodiment is preferably 0.2～1.2wt.%, and the polymerization degree is preferably 20～50.
Alkynol class inhibitor described in embodiment is preferably to mix in 1: 1～5: 1 by ethynyl-1-hexalin and 2-methyl-3-butyne-2-alcohol in mass ratio.
Silicon-dioxide described in embodiment is aerosil or precipitated silica, and the specific surface area of described aerosil is preferably 150～400m
2/ g, the specific surface area of described precipitated silica is preferably 150～220m
2/ g.
Fire retardant described in embodiment is preferably any one or the mixture more than two kinds in aluminium hydroxide, antimonous oxide, TDE, decabromodiphynly oxide, mica powder.
Polysiloxane I described in embodiment is the tetrem thiazolinyl first divinyl disiloxane by the octamethylcyclotetrasiloxane of 100 mass parts, 0.2～0.5 mass parts, under the katalysis of silanol potassium, in 140 ℃ of constant temperature polymerizations 4 hours, then use in carbonic acid gas and 2 hours, be warmed up to again 180 ℃, deviate from low-molecular material and prepare and get under the vacuum condition of 500 pools.
Polysiloxane II described in embodiment is by the tetrem thiazolinyl first divinyl disiloxane of the octamethylcyclotetrasiloxane of 100 mass parts, 0.1～0.2 mass parts, the tetramethyl-of 10～30 mass parts-tetrem thiazolinyl cyclotetrasiloxane, under the katalysis of silanol potassium, in 140 ℃ of constant temperature polymerizations 4 hours, then use in carbonic acid gas and 2 hours, be warmed up to again 180 ℃, deviate from low-molecular material and prepare and get under the vacuum condition of 500 pools.
Polysiloxane III described in embodiment is the tetrem thiazolinyl first divinyl disiloxane by the octamethylcyclotetrasiloxane of 100 mass parts, 0.2 mass parts, the tetramethyl-of 8 mass parts-tetrem thiazolinyl cyclotetrasiloxane, under the katalysis of silanol potassium, in 140 constant temperature polymerization 4 hours, then use in carbonic acid gas and 2 hours, be warmed up to again 180 ℃, deviate from low-molecular material and prepare and get under the vacuum condition of 500 pools.
Hydrogen containing siloxane described in embodiment is to be formed by tetramethyl-ring tetrasiloxane, tetramethyl disiloxane or full containing hydrogen silicone oil and DMC pre-polymerization under the Zeo-karb effect of wide aperture; Temperature of reaction is 40～60 ℃, and the reaction times is 2～6 hours, and after reaction finished and restraints, the elimination Zeo-karb was warmed up to 140～160 ℃, and vacuum deviates to hang down sub-thing, and get final product.For example, prepare by full containing hydrogen silicone oil and DMC the operation that hydrogen content is 0.8%, viscosity is the 60cs hydrogen containing siloxane as follows: add the DMC of 100 mass parts, the full containing hydrogen silicone oil of 100 mass parts and the wide aperture Zeo-karb of 20 mass parts in vial, be warmed up to 40 ℃, after insulation reaction 4 hours, the elimination Zeo-karb, then be warmed up to 140 ℃, pass into nitrogen, vacuum is deviate from residual low-molecular material, namely gets target compound.
Be necessary at last to be pointed out that at this: above content only is used for the present invention is described in further detail; can not be interpreted as limiting the scope of the invention, some nonessential improvement and adjustment that those skilled in the art makes according to foregoing all belong to protection scope of the present invention.
Claims (10)
1. anti-flaming liquid silicon rubber is used in filamentary material coating, it is characterized in that: be to form in 1: 10～10: 1 in mass ratio by A component and B component; Wherein,
The compositing formula of A component is as follows:
Base glue 100 mass parts
Platinum complex compound 0.2～1.0 mass parts
Tackifier 0.2～5.0 mass parts;
The compositing formula of B component is as follows:
The compositing formula of described basic glue is as follows:
Above-mentioned per-cent is mass percent, and the mass percent sum of described composition is 100%; Described polysiloxane I is that the viscosity 25 ℃ of mensuration is that 5000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.25～0.5wt.%; Described polysiloxane II is that the viscosity 25 ℃ of mensuration is that 1500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.0wt.%; Described polysiloxane III is that the viscosity 25 ℃ of mensuration is that 250～1500cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 1～10wt.%; The composition general formula of the organopolysiloxane of described ethenyl blocking is: R
2SiO (SiRR ' O)
nSiR
2, R wherein is vinyl, R ' is vinyl or methyl.
2. anti-flaming liquid silicon rubber is used in filamentary material coating according to claim 1, and it is characterized in that: described platinum complex compound is to be formed by Platinic chloride and divinyl dimethyl sily oxide, and platinum content wherein is 1000～5000ppm.
3. anti-flaming liquid silicon rubber is used in filamentary material according to claim 1 coating, it is characterized in that: described tackifier are selected from any one or the mixture more than two kinds in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-aminopropyl triethoxysilane.
4. anti-flaming liquid silicon rubber is used in filamentary material coating according to claim 1, and it is characterized in that: the hydrogen content in described hydrogen containing siloxane is 0.2～1.2wt.%, and the polymerization degree is 20～50.
5. anti-flaming liquid silicon rubber is used in filamentary material according to claim 1 coating, it is characterized in that: described alkynol class inhibitor is to be to mix in 1: 1～5: 1 in mass ratio by ethynyl-1-hexalin and 2-methyl-3-butyne-2-alcohol.
6. anti-flaming liquid silicon rubber is used in filamentary material coating according to claim 1, it is characterized in that: described silicon-dioxide is aerosil or the precipitated silica after silane coupling agent is done the hydrophobic processing.
7. anti-flaming liquid silicon rubber is used in filamentary material according to claim 1 coating, it is characterized in that: described fire retardant is selected from any one or the mixture more than two kinds in aluminium hydroxide, antimonous oxide, TDE, decabromodiphynly oxide, mica powder.
8. anti-flaming liquid silicon rubber is used in filamentary material coating according to claim 7, it is characterized in that: described fire retardant is made hydrophobic through silane coupling agent and is processed.
9. according to claim 6 or 8 described filamentary materials are coated with and use anti-flaming liquid silicon rubbers, it is characterized in that: describedly make hydrophobic through silane coupling agent and process, refer to object being treated and silane coupling agent be in mass ratio mixed in 5: 1～10: 1 after, 120～130 ℃ of stirring reactions 5～7 hours; Described silane coupling agent is selected from any one or the mixture more than two kinds in hexamethyldisilazane, dimethyldiethoxysilane, dimethyldimethoxysil,ne, dimethyldichlorosilane(DMCS), dimethyl cyclosiloxane.
10. a filamentary material claimed in claim 1 is coated with the preparation method who uses anti-flaming liquid silicon rubber, it is characterized in that, comprises the steps:
A) prepare basic glue
1. the polysiloxane I of 80～100% formula ratios and polysiloxane II, silicon-dioxide and the fire retardant of formula ratio are added in kneader, at room temperature mediated 1～2 hour;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1～2 hour;
3. vacuumize, continue to mediate 2～4 hours in 150～160 ℃ under vacuum condition, then stop vacuumizing, be cooled to 110～130 ℃, add the polysiloxane I of remaining formula ratio and the polysiloxane III of formula ratio, mix, namely get described basic glue;
B) preparation A component
Get basic glue 100 mass parts, then add platinum complex compound and the tackifier of formula ratio, mix, namely get described A component;
C) preparation B component
Get basic glue 100 mass parts, then add hydrogen containing siloxane, alkynol class inhibitor and the tackifier of formula ratio, mix, namely get described B component;
D) be to mix in 1: 10～10: 1 in mass ratio with the A component that makes and B component, namely get described filamentary material coating anti-flaming liquid silicon rubber.
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| CN104945909A (en) * | 2015-06-30 | 2015-09-30 | 烟台金润消防工程有限公司 | Medium-density silicone rubber for nuclear power |
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