CN103044922A - Halogen-free flame retardant, high-temperature resisting and rapidly solidified deacetone silicon rubber and preparation method thereof - Google Patents
Halogen-free flame retardant, high-temperature resisting and rapidly solidified deacetone silicon rubber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free flame retardant, high-temperature resisting and rapidly solidified deacetone silicon rubber and a preparation method thereof. Hydroxy-end-capped polydimethylsiloxane is used as the main body and is compounded with a thermal-resisting additive and a flame retardant additive, wherein the halogen-free flame retardant, high-temperature resisting and rapidly solidified deacetone silicon rubber comprises the following ingredients by weight: 100 parts of the hydroxy-end-capped polydimethylsiloxane serving as a main body, 1-50 parts of polydimethylsiloxane, 5-18 parts of silicon oxide, 5-15 parts of thermal-resisting additive, 50-200 parts of flame retardant additive, 0.5-2.5 parts of tackifier, 0.5-1 part of organic guanidine catalyst and 5-8 parts of deacetone siloxane cross-linking agent; the thermal-resisting additive is one or a mixture of several of iron oxide red, cerium oxide of which the purity is not less than 90% and tin oxide of rutile structure; and the flame retardant additive is one or a mixture of several of aluminum hydroxide, magnesium hydrate, zinc borate, phosphate ester, phosphonate, phosphine oxide and organic phosphorus. The deacetone silicon rubber has good thermal resistance, flame retardant effect and mechanical properties at 250-300 DEG C, and is simple in preparation method and high in production efficiency.
Description
Technical field
The present invention relates to a kind of room temperature vulcanized silicone rubber, relate in particular to a kind of deacetone room temperature vulcanized silicone rubber and preparation method thereof.
Background technology
Single-component room temperature vulcanized (hereinafter to be referred as RTV-1) silicon rubber has good heat-resisting, anti-weather aging, moisture-proof and permeability, and the performances such as excellent electrical property and unreactiveness, in aviation, electronics, automobile, machinery, instrument and health care and daily life, obtain to use widely.RTV-1 silicon rubber can keep elasticity for a long time in extremely wide temperature range (-60 ~ 200 ℃), itself has excellent resistance to elevated temperatures, but the progress along with modern science and technology, its thermotolerance is had higher requirement, as: the function of electronic product is become stronger day by day, this just requires electronic devices and components towards high-power, high integrated, small volume future development, the elements such as the chip that many electrical equipment are used, electric capacity, resistance criticize cover, silicon rubber that sealing, embedding are used is at 250 ℃ of life-time service; Especially along with the development of Aeronautics and Astronautics technology, especially thermotolerance has been had higher requirement, the thermotolerance that further improves RTV-1 silicon rubber gluing glue becomes study hotspot.
RTV-1 silicon rubber is in the application in various fields, especially in the electronic industry, applied environment usually is in high pressure occasion shelf depreciation, sparking and easily forms disaster hidden-trouble, this not only requires tackiness agent heat-resisting better, and is also more and more higher to the requirement of flame retardant resistance, cementability and the electrical property of tackiness agent simultaneously.The flame retardant resistance of tackiness agent and the composition of sizing material have very large relation, and adding fire retardant in sizing material also is a kind of effectively method.The flame retarding efficiency of halogen flame is high, moderate cost, but the hydrogen halide that discharges during the halogen flame burning is not only poisonous and have corrodibility, and can produce a large amount of smog.Because the increase of environmental consciousness, and environmental regulation is to the restriction of halogen flame, and halogen-free anti-flaming silicon rubber is paid close attention in recent years widely, and makes some progress.
Flame-retardant silicone mainly contains ketoxime removing type, dealcoholizing-type and deacetone.The ketoxime removing type flame retardant silica gel has corrosion to copper, has limited its use range.The factors such as dealcoholizing-type flame retardant silica gel curing speed is slow, and storage period is short are restricted in the demanding occasion of technique beat.Simultaneously, ketoxime type and dealcoholizing-type flame retardant silica gel resistance toheat are poor, and general heat resisting temperature at high temperature uses to be restricted about 150 ℃.Deacetone flame retardant silica gel system curing speed is fast, and neutral curing can not used poisonous organotin catalysts, and bonding strength is high, excellent storage stability, and the high-temperature resistant result excellence becomes the trend of high-end flame-retardant silicone.
At present, domestic flame-retardant silicone is in the majority with dealcoholizing-type generally, higher level have soon solid, heat-resisting (250 ~ 300 ℃) concurrently, it is fire-retardant that (FV-1 ~ FV-0) silicone rubber products is not yet seen.Abroad, Japan XINYUE develops flame retardant type and takes off acetone liquid silastic KE-3424G, KE3494, KE3490, has commercially obtained preferably and has used, but expensive, it is also untimely to supply.
Provide a kind of raw material to be easy to get, the suitable and performance of price can be taken off the product that acetone liquid silastic KE-3424G, KE3494, KE3490 etc. compare favourably with flame retardant type becomes study hotspot for this reason.
Summary of the invention
The present invention is directed to the deficiency of present technology, a kind of halogen-free flame-retardant, high temperature resistant, quick-setting acetone-removing silicon rubber and preparation method thereof are provided, make product have high heat resistance energy (250 ~ 300 ℃), flame retardant resistance (FV-0), this glue vulcanization rate is fast, do not use the poisonous catalyzer such as organotin, organic titanium, and be neutral curing, to the base material non-corrosiveness.
The scheme that the present invention solves the problems of the technologies described above is as follows: a kind of halogen-free flame-retardant, high temperature resistant, quick-setting acetone-removing silicon rubber are comprised of each starting material of following weight proportion:
100 parts of hydroxy-end capped polydimethylsiloxanes
1 ~ 50 part of polydimethylsiloxane
5 ~ 18 parts of silicon-dioxide
5 ~ 15 parts of heat-resisting additives
50 ~ 200 parts of flame-retardant additives
0.5 ~ 2.5 part of tackifier
0.5 ~ 1 part of organic guanidine catalyst
5 ~ 8 parts of deacetone siloxane crosslinkers
Wherein, described hydroxy-end capped polydimethylsiloxane is that range of viscosities is a kind of in the siloxanes of 4000 ~ 80000cps or any several mixture, and described hydroxy-end capped polydimethylsiloxane structural formula is:
R is CH
3-, CH
3CH
2-or phenyl;
Described polydimethylsiloxane claims again dimethyl silicone oil or silicone oil, for range of viscosities is a kind of among 50 ~ 2000cps or any several mixture;
Described heat-resisting additive is a kind of or any several mixture in red iron oxide, cerium oxide, the stannic oxide, and wherein, the purity of described cerium oxide is for being not less than 90%, and the impurity such as cupric oxide, zinc oxide are not more than 10%; Described stannic oxide is the characteristics such as nano level belongs to rutile structure, and its Heat stability is good and stable mechanical performance performance are good;
Described flame-retardant additive be aluminium hydroxide, magnesium hydroxide, zinc borate, phosphoric acid ester, phosphonic acid ester, phosphine oxide, organophosphorated salt, in a kind of or any several mixture, wherein, described aluminium hydroxide, magnesium hydroxide and zinc borate are through surface-treated or without surface-treated, preferably through surface-treated.
When at high temperature (250 ~ 300 ℃) use, selected halogen-free flame retardants requires fire retardant that preferably thermostability is arranged, the thermostability of aluminium hydroxide is relatively poor, and magnesium hydroxide, zinc borate have preferably thermostability, at high temperature still have good flame retardant resistance, so preferred fire retardant is through surface-treated magnesium hydroxide and zinc borate powder.
On the such scheme basis, described surface treatment refers to: the hexa methyl silazane of 1 ~ 15% weight ratio and 85% ~ 99% magnesium hydroxide or aluminium hydroxide or zinc borate powder are added in the reactor then warming while stirring, pressure treatment and get.
On the such scheme basis, described hydroxyl endblocked polydimethylsiloxane is called again 107, and the viscosity preferred viscosity ranges is 5000 ~ 10000mPas, and being more preferably range of viscosities is 6000 ~ 8000mPas.
On the such scheme basis, described polydimethylsiloxane range of viscosities preferred viscosity ranges is 50 ~ 200mPas.
Described silicon-dioxide is Fumed silica, and its specific surface area is 50 ~ 400m
2/ g.
Described viscosity increaser is γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, 3-aminopropyl methyl dimethoxy oxygen base γ, 3-aminopropyl methyldiethoxysilane, the phenylamino Union carbide A-162, the 3-(methacryloxy) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, N-(β-aminoethyl)-γ-aminopropyl dimethoxy silane, γ-[(2,3)-and epoxypropyl] propyl trimethoxy silicane, γ-[(2,3)-epoxypropyl] propyl group dimethoxy silane, the isocyanic acid propyl-triethoxysilicane, the 3-mercaptopropyltriethoxysilane, the mixture of one or more in the 3-mercaptopropyl trimethoxysilane.
Described organic guanidine catalyst is 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane or 1,1,3,3-tetramethyl-guanidine radicals propyl-triethoxysilicane.
Described deacetone siloxane crosslinker is that one or more mixture and phenyl three (different propenyloxy group) silane mixture of methyl three (different propenyloxy group) silane, four (different propenyloxy group) silane, chloromethyl three (different propenyloxy group) silane, vinyl three (different propenyloxy group) silane obtains, and wherein the blending ratio of the former with the latter is 1:6 ~ 6:1.
The present invention puies forward the preparation method who states above-mentioned halogen-free flame-retardant, high temperature resistant, quick-setting acetone-removing silicon rubber, realizes by following steps:
Step 1: count by weight, 100 parts hydroxy-end capped polydimethylsiloxanes, 1 ~ 50 part polydimethylsiloxane, 5 ~ 18 parts Fumed silica, 5 ~ 15 parts heat-resisting additive powder, 50 ~ 200 parts flame-retardant additive powder are joined in the kneader, and mixing dehydration 30 ~ 360 minutes in 110 ~ 180 ℃ of temperature, after the cooling base-material is for subsequent use;
Step 2: at room temperature, base-material is joined in the double-planet stirrer, add 5 ~ 8 parts of cross-linked rubbers, add 0.5 ~ 2.5 part tackifier and organic guanidine catalyst of 0.5 ~ 1 part behind vacuum stirring 10 ~ 60min, the discharging sealing is preserved behind vacuum stirring 10 ~ 60min.
The present invention has selected and has taken off the acetone system and add heat-resisting additive to improve the thermostability of product, by adding fire retardant additive without halogen to improve the flame retarding efficiency of product, makes product have the soon performances such as solid, heat-resisting (250 ~ 300 ℃), fire-retardant (FV-0) concurrently simultaneously.
Owing to adopted technique scheme, a kind of halogen-free flame-retardant of the present invention, high temperature resistant, quick-setting acetone-removing silicon rubber have the following advantages:
One, the acetone system is taken off in employing, and curing speed is fast, widely cementability;
Two, utilize Fumed silica as reinforced filling, higher mechanical property is arranged;
Three, by adding heat-resisting additive (red iron oxide, cerium oxide or stannic oxide), make silicon rubber have good thermostability;
Four, the present invention processes magnesium hydroxide or aluminium hydroxide or zinc borate powder by adding nitrogenous hexa methyl silazane, the flame retardant effect that produces is greatly improved, flame retardant effect all can reach the FV-0 level, the avidity of powder and polymkeric substance significantly improves after the modification, the larger improvement of the mechanical property of product and mechanical property;
Five, the preparation method of sealing glue is simple, and production unit is conventional equipment, and produces environmental friendliness in the production process without the three wastes.
Halogen-free flame-retardant provided by the invention, high temperature resistant, quick-setting acetone-removing silicon rubber, basic mechanical design feature index such as following table:
Embodiment
Below in conjunction with embodiment, further illustrate the present invention, but embodiments of the present invention are not limited to this.
Embodiment 1
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 6000mPas) 100 weight parts, surface-treated magnesium hydroxide 100 weight parts, surface-treated zinc borate 20 weight parts, White Carbon black 8 weight parts, red iron oxide 10 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, add methyl three (different propenyloxy group) silane 2 weight parts, phenyl three (different propenyloxy group) silane 6 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, add γ-aminopropyl triethoxysilane 1 weight part, 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane, 0.6 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
Embodiment 2
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 8000mPas) 100 weight parts, surface-treated magnesium hydroxide 120 weight parts, surface-treated zinc borate 20 weight parts, White Carbon black 8 weight parts, red iron oxide 10 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, add chloromethyl three (different propenyloxy group) silane 4 weight parts, phenyl three (different propenyloxy group) silane 4 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, add N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 1 weight part, 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane, 0.7 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
Embodiment 3
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 10000mPas) 100 weight parts, surface-treated magnesium hydroxide 120 weight parts, surface-treated zinc borate 20 weight parts, White Carbon black 10 weight parts, nano-cerium oxide 8 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, add chloromethyl three (different propenyloxy group) silane 4 weight parts, phenyl three (different propenyloxy group) silane 4 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, add γ-[(2,3)-and epoxypropyl] propyl trimethoxy silicane 1 weight part, 1,1,3,3-tetramethyl-guanidine radicals propyl-triethoxysilicane 0.8 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
Embodiment 4
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 8000mPas) 100 weight parts, surface-treated magnesium hydroxide 120 weight parts, surface-treated zinc borate 20 weight parts, White Carbon black 8 weight parts, nano tin dioxide (rutile structure) 8 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, add four (different propenyloxy group) silane, 6 weight parts, phenyl three (different propenyloxy group) silane 2 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, add γ-aminopropyl triethoxysilane 0.5 weight part, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 0.5 weight part, 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane 0.8 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
Embodiment 5
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 8000mPas) 100 weight parts, surface-treated magnesium hydroxide 120 weight parts, surface-treated zinc borate 20 weight parts, White Carbon black 8 weight parts, red iron oxide 5 weight parts, nano tin dioxide (rutile structure) 4 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, and base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, add chloromethyl three (different propenyloxy group) silane 4 weight parts, phenyl three (different propenyloxy group) silane 4 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, adding 3-(methacryloxy) propyl trimethoxy silicane is 0.5 part, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 1 weight part, 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane 0.7 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
Embodiment 6
With hydroxy-end capped polydimethylsiloxane (25 ℃ time viscosity be 10000mPas) 100 weight parts, surface-treated magnesium hydroxide 140 weight parts, surface-treated zinc borate 30 weight parts, White Carbon black 8 weight parts, red iron oxide 10 weight parts join in the kneader in 120 ℃ of temperature, mixing dehydration 240 minutes, base-material is for subsequent use after the cooling; Base-material is joined in the double-planet stirrer, enter four (different propenyloxy group) silane, 6 weight parts, phenyl three (different propenyloxy group) silane 2 weight parts, vacuumize stir 20 ~ 30min(vacuum tightness for-more than the 0.095MPa) after, add the 3-(methacryloxy) 1.5 parts of propyl trimethoxy silicanes, 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane, 0.8 weight part, vacuumize stir 20 ~ 30min after the discharging sealing preserve.
The halogen-free flame-retardant that other component of the present invention and proportioning consist of, high temperature resistant, quick-setting acetone-removing silicon rubber all in protection domain of the present invention, are described explanation at this no longer one by one.
The above embodiment is only in order better to illustrate the present invention, and is not limited to scope of the present invention, and is within the spirit and principles in the present invention all, all any modifications, is equal to replacement, improvement etc., all falls within the scope of protection of the present invention.
Claims (8)
1. a halogen-free flame-retardant, high temperature resistant, quick-setting acetone-removing silicon rubber take hydroxy-end capped polydimethylsiloxane as main body, cooperate with heat-resisting additive and flame-retardant additive, it is characterized in that, take by weighing following component according to parts by weight:
100 parts of hydroxy-end capped polydimethylsiloxanes
1 ~ 50 part of polydimethylsiloxane
5 ~ 18 parts of silicon-dioxide
5 ~ 15 parts of heat-resisting additives
50 ~ 200 parts of flame-retardant additives
0.5 ~ 2.5 part of tackifier
0.5 ~ 1 part of organic guanidine catalyst
5 ~ 8 parts of deacetone siloxane crosslinkers
Wherein, described hydroxy-end capped polydimethylsiloxane is that range of viscosities is a kind of in the siloxanes of 4000 ~ 80000cps or any several mixture, and described hydroxy-end capped polydimethylsiloxane structural formula is:
R is CH
3-, CH
3CH
2-or phenyl;
Described polydimethylsiloxane (silicone oil) is a kind of among 50 ~ 2000cps or any several mixture for range of viscosities;
Described heat-resisting additive is a kind of or any several mixture in red iron oxide, cerium oxide, the stannic oxide, and wherein, the purity of described cerium oxide is not less than 90%, and cupric oxide, zinc oxide content are not more than 10%; Described stannic oxide belongs to rutile structure;
Described flame-retardant additive be aluminium hydroxide, magnesium hydroxide, zinc borate, phosphoric acid ester, phosphonic acid ester, phosphine oxide, organophosphorated salt, in a kind of or any several mixture;
Wherein said aluminium hydroxide, magnesium hydroxide and zinc borate are through surface-treated or without surface-treated.
2. halogen-free flame-retardant according to claim 3, high temperature resistant, quick-setting acetone-removing silicon rubber, it is characterized in that, described surface treatment refers to the hexa methyl silazane of 1 ~ 15% weight ratio and 85% ~ 99% magnesium hydroxide or aluminium hydroxide or zinc borate powder are added in the reactor, then warming while stirring, pressure treatment and get.
3. halogen-free flame-retardant according to claim 1, high temperature resistant, quick-setting acetone-removing silicon rubber is characterized in that, described organic guanidine catalyst is 1,1,3,3-tetramethyl-guanidine radicals propyl trimethoxy silicane or 1,1,3,3-tetramethyl-guanidine radicals propyl-triethoxysilicane.
4. halogen-free flame-retardant according to claim 1, high temperature resistant, quick-setting acetone-removing silicon rubber, it is characterized in that described deacetone siloxane crosslinker is that one or more mixture and phenyl three (different propenyloxy group) silane mixture of methyl three (different propenyloxy group) silane, four (different propenyloxy group) silane, chloromethyl three (different propenyloxy group) silane, vinyl three (different propenyloxy group) silane obtains.
5. halogen-free flame-retardant according to claim 1, high temperature resistant, quick-setting acetone-removing silicon rubber, it is characterized in that, described viscosity increaser is γ-aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, 3-aminopropyl methyl dimethoxy oxygen base γ, 3-aminopropyl methyldiethoxysilane, the phenylamino Union carbide A-162, the 3-(methacryloxy) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl triethoxysilane, N-(β-aminoethyl)-γ-aminopropyl dimethoxy silane, γ-[(2,3)-and epoxypropyl] propyl trimethoxy silicane, γ-[(2,3)-epoxypropyl] propyl group dimethoxy silane, the isocyanic acid propyl-triethoxysilicane, the 3-mercaptopropyltriethoxysilane, the mixture of one or more in the 3-mercaptopropyl trimethoxysilane.
6. halogen-free flame-retardant according to claim 1, high temperature resistant, quick-setting acetone-removing silicon rubber is characterized in that, described silicon-dioxide is Fumed silica, and its specific surface area is 50 ~ 400m
2/ g.
7. the manufacture method of halogen-free flame-retardant according to claim 1, high temperature resistant, quick-setting acetone-removing silicon rubber the steps include:
The preparation of base-material
Hydroxy-end capped polydimethylsiloxane, heat-resisting additive powder, flame-retardant additive powder, silicon-dioxide powdery are joined in the kneader, and mixing dehydration 30 ~ 360 minutes in 110 ~ 180 ℃ of temperature, after the cooling base-material;
Seal gum is synthetic
At room temperature, base-material is joined in the stirrer, again polydimethyl silane, linking agent, silane viscosity increaser, catalyzer are joined in the stirrer and stir with base-material, vacuum tightness is 0.6 ~ 0.1MPa, reacted 0.5 ~ 5 hour, and made halogen-free flame-retardant, high temperature resistant, quick-setting acetone-removing silicon rubber.
8. the manufacture method of halogen-free flame-retardant according to claim 7, high temperature resistant, quick-setting acetone-removing silicon rubber is characterized in that adopting planetary mixer when described silicon rubber is synthetic, and stirring velocity is 20 ~ 100 rev/mins.
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