CN103305012A - One-component addition type liquid silicone rubber and preparing method thereof - Google Patents
One-component addition type liquid silicone rubber and preparing method thereof Download PDFInfo
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Abstract
The invention discloses one-component addition type liquid silicone rubber and a preparing method thereof. The one-component addition type liquid silicone rubber is formed by basic rubber, modified additives, platinum complexes, hydrogen-containing polysiloxane and alkynol inhibitors according to a certain ratio, wherein the basic rubber is formed by organic polysiloxanes and hydrophobic silicon dioxide with different viscosities and vinyl contents at the vinyl sealing end. The preparing method includes basic rubber preparing and liquid silicone rubber preparing. The liquid silicone rubber is ultra-low in viscosity, good in flowing property, strong in adhesion, convenient to use, easy to operate and good in storage stability. The preparing method is simple, practical, low in cost and applicable to large-scale production and has an industrial application value.
Description
Technical field
The present invention relates to the organic silicon rubber material technical field, be specifically related to a kind of single-component add-on type liquid silicon rubber and preparation method thereof.
Background technology
Because silicon rubber has excellent ageing-resistant performance, electrical insulating property and better mechanical strength, is widely used in various industries.Common silicon rubber is only applicable to make the prefabricated components such as regular wear ring, sealing-ring, sealed strip, this accessory assembling trouble, and do not have cementability, use extremely inconvenient, because liquid silastic has the processing characteristics of excellent flowability, excellence with respect to firm silicone rubber, more flexible under different working conditionss, quicker.Thereby if can research and develop a kind of good flowing properties, cementability is strong, the liquid silastic of easy to use, easy to operate, excellent storage stability is worth significant and widespread use.
Summary of the invention
The problems referred to above and demand for prior art exists the purpose of this invention is to provide a kind of single-component add-on type liquid silicon rubber and preparation method thereof, to satisfy the widespread use requirement of silastic material.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of single-component add-on type liquid silicon rubber consists of according to the mass fraction:
The compositing formula of described basic glue is as follows, by mass percentage:
Polysiloxane I 30～70%
Polysiloxane II 4～30%
Water drain silica 20～40%;
Wherein, described polysiloxane I is that the viscosity 25 ℃ of mensuration is that 500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.5mol.%; Described polysiloxane II is that the viscosity 25 ℃ of mensuration is that 8000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 2.5～5.0mol.%; The composition general formula of the organopolysiloxane of described ethenyl blocking is: R
2SiO (SiRR ' O) nSiR
2, wherein R is vinyl, R ' is vinyl or methyl.
Further, described platinum complex compound is synthetic by Platinic chloride and Virahol coordination, and platinum content wherein is 500～3000ppm.
Further, described hydrogen containing siloxane is to be 0.1-0.25mol.% by hydrogen content, viscosity is that end hydrogen based polysiloxane and the hydrogen content of 20-50 centipoise is 0.5-0.75mol.%, and viscosity is that the side group hydrogen containing siloxane of 20-50 centipoise forms for the ratio cooperation of 3-9:1 in mass ratio.
Further, described alkynol class inhibitor is that encircling pure by heptamethylcyclotetrasiloxane and ethynyl-1-is 1-2:1 composite modified forming under the Platinic chloride effect by the mole mass ratio.
Further, described property-modifying additive comprise in the concentrated dispersion liquid of cerous oxide, zirconium dioxide, ferric oxide, nanometer polytetrafluoroethylcomposite powder, tetrafluoroethylene, silane coupling agent, titanate coupling agent, the aluminate coupling agent any one or multiple.
Further, described water drain silica is aerosil or the precipitated silica after silane coupling agent is done the hydrophobic processing.
The preparation method of above-mentioned single-component add-on type liquid silicon rubber comprises the steps:
A, prepare basic glue:
1. the polysiloxane I of 50～100% formula ratios, the water drain silica of formula ratio are added in the kneader, at room temperature mediated 2～4 hours;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1～2 hour;
3. vacuumize, under vacuum condition, continue to mediate 2～4 hours in 150～160 ℃, then stop to vacuumize, be cooled to 110～130 ℃, add the polysiloxane I of remaining formula ratio and the polysiloxane II of formula ratio, mix, namely get described basic glue;
Hydrogen containing siloxane, the alkynol class inhibitor of b, basic glue 100 mass parts of getting above-mentioned preparation, adding formula ratio stir, the platinum complex compound, the property-modifying additive that add formula ratio mix again, and vacuumize and namely get described single-component add-on type liquid silicon rubber.
Beneficial effect of the present invention:
1, liquid silastic of the present invention only has the viscosity of 2000-10000 centipoise, has splendid flowability, can place more than 1 year at 25 ℃ of air-tight states, construct during use in substrate surface, just solidify fully with 150-200 ℃ of 300min, silica gel after the curing has good mechanical property, and various base materials are had stronger cementability.
2, liquid silastic of the present invention can be used for bonding, production machinery gasket of material etc.100ml, 300ml, 600ml hard tube or hose packing be can make, 20L, the encapsulation of 200L standard broad mouth bucket also can be used, easy to use, be widely used, applied widely.
3, liquid silastic preparation method of the present invention is simple, with low cost, is fit to large-scale production, has industrial application value.
Embodiment
Below in conjunction with embodiment the present invention is done further explanation.The following example only is used for explanation the present invention, but is not used for limiting practical range of the present invention.
A kind of single-component add-on type liquid silicon rubber consists of according to the mass fraction:
The compositing formula of described basic glue is as follows, by mass percentage:
Polysiloxane I 30～70%
Polysiloxane II 4～30%
Water drain silica 20～40%;
Wherein, described polysiloxane I is that the viscosity 25 ℃ of mensuration is that 500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.5mol.%; Described polysiloxane II is that the viscosity 25 ℃ of mensuration is that 8000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 2.5～5.0mol.%; The composition general formula of the organopolysiloxane of described ethenyl blocking is: R
2SiO (SiRR ' O) nSiR
2, wherein R is vinyl, R ' is vinyl or methyl.
The described polysiloxane I of embodiment preparation method is: by the octamethylcyclotetrasiloxane of 100 mass parts, the tetramethyl divinyl disiloxane of 0.5-0.8 mass parts, under the Tetramethylammonium hydroxide katalysis, in 100 ℃ of constant temperature polymerizations 2.5 hours, then be warmed up to 150 ℃ of balances 1 hour, be warmed up to again 180 ℃, deviate from low-molecular material under the vacuum condition of 200 pools, namely preparing and getting viscosity is that 500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.5mol.%.
The preparation method of the described polysiloxane II of embodiment is: by the octamethylcyclotetrasiloxane of 100 mass parts, the tetrem thiazolinyl first divinyl disiloxane of 0.2～0.3 mass parts, under the katalysis of tetramethyl-hydrogen-oxygen ammonium, in 100 ℃ of constant temperature polymerizations 2.5 hours, then be warmed up to 150 ℃ of balances 1 hour, be warmed up to again 180 ℃, deviate from low-molecular material under the vacuum condition of 200 pools, preparing and getting viscosity is that 8000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 2.5～5.0mol.%.
Described platinum complex compound is synthetic by Platinic chloride and Virahol coordination, and platinum content wherein is 500～3000ppm.The described platinum complexes preparation of embodiment method is: add 5 gram chloroplatinic acid hydrate and 200ml Virahols in the 500ml four-hole bottle, temperature rising reflux is 1 hour under logical nitrogen.Add dried over sodium sulfate after the cooling, then the solid slag of elimination repeatedly washes with Virahol solid slag, and scavenging solution is added in the filtrate, namely makes the platinum catalyst solution of Virahol coordination.
Described hydrogen containing siloxane is to be 0.1-0.25mol.% by hydrogen content, viscosity is that end hydrogen based polysiloxane and the hydrogen content of 20-50 centipoise is 0.5-0.75mol.%, and viscosity is that the side group hydrogen containing siloxane of 20-50 centipoise forms for the ratio cooperation of 3-9:1 in mass ratio.The preparation method that the described hydrogen content of embodiment is 0.75%, viscosity is the side group hydrogen containing siloxane of 50 centipoises is: the dimethyl siloxane mixed methylcyclosiloxane (DMC), the containing hydrogen silicone oil of 100 mass parts and the wide aperture Zeo-karb of 20 mass parts that add 100 mass parts in vial, be warmed up to 40 ℃, after the insulation reaction 4 hours, the elimination Zeo-karb, be warmed up to again 140 ℃, pass into nitrogen, vacuum is deviate from residual low-molecular material, namely gets target compound.Adjust the quality of containing hydrogen silicone oil and DMC, same preparation method prepares the side group hydrogen containing siloxane of different hydrogen contents and viscosity.Hydrogen content is 0.1-0.25mol.%, and viscosity is that the end hydrogen based polysiloxane of 20-50 centipoise is by DMC, tetramethyl disiloxane and wide aperture Zeo-karb, makes with same preparation method.
Described alkynol class inhibitor is that encircling pure by heptamethylcyclotetrasiloxane and ethynyl-1-is 1-2:1 composite modified forming under the Platinic chloride effect by the mole mass ratio.
Described property-modifying additive is to add subsidiary material not of the same race according to the Application Areas of sizing material, as: when heat-resisting the requirement arranged, need to add the high temperature materials such as cerous oxide, zirconium dioxide, ferric oxide; When the oil resistant requirement is arranged, need to add the oil resisting materials such as nanometer polytetrafluoroethylcomposite powder or the concentrated dispersion liquid of tetrafluoroethylene; When having pair metal that bonding requirements is arranged, need to add with the silane coupling agent of epoxy group(ing) or titanic acid ester, aluminate coupling agent; When having pair organic high molecular polymer that bonding requirements is arranged, need to add the silane coupling agent with propenyl, epoxy group(ing), vinyl.
Described water drain silica is aerosil or the precipitated silica after silane coupling agent is done the hydrophobic processing.The described water drain silica of embodiment is to be the R972 water drain silica by the trade mark that Degussa company provides.
The preparation method of above-mentioned single-component add-on type liquid silicon rubber comprises the steps:
A, prepare basic glue:
1. the polysiloxane I of 50～100% formula ratios, the water drain silica of formula ratio are added in the kneader, at room temperature mediated 2～4 hours;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1～2 hour;
3. vacuumize, under vacuum condition, continue to mediate 2～4 hours in 150～160 ℃, then stop to vacuumize, be cooled to 110～130 ℃, add the polysiloxane I of remaining formula ratio and the polysiloxane II of formula ratio, mix, namely get described basic glue;
Hydrogen containing siloxane, the alkynol class inhibitor of b, basic glue 100 mass parts of getting above-mentioned preparation, adding formula ratio stir, the platinum complex compound, the property-modifying additive that add formula ratio mix again, and vacuumize and namely get described single-component add-on type liquid silicon rubber.
Liquid silastic of the present invention only has the viscosity of 2000-10000 centipoise, has splendid flowability, can place more than 1 year at 25 ℃ of air-tight states, construct during use in substrate surface, just solidify fully with 150-200 ℃ of 300min, silica gel after the curing has good mechanical property, and various base materials are had stronger cementability.
Embodiment 1
A, prepare basic glue
1. adding 140kg viscosity in the 500L kneader is that 1000cp (25 ℃), contents of ethylene are the polysiloxane I of 1.2mol.%, and the aerosil of 100kg 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 1 hour;
3. being evacuated to vacuum tightness is 0.8MPa, under vacuum condition, continue to mediate 3 hours in 150～160 ℃, then stop to vacuumize, be cooled to 120 ℃, the polysiloxane I and the 16kg viscosity that add 100kg viscosity and be 1000cp (25 ℃), contents of ethylene and be 1.2mol.% are that 10000cp (25 ℃), contents of ethylene are the polysiloxane II of 5.0mol.%, mix, namely get described basic glue;
B, preparation single-component add-on type liquid silicon rubber
In the 300L planetary mixer, add the basic glue of the above-mentioned preparation of 200kg, hydrogen containing siloxane and the 0.08kg alkynol class inhibitor that 4.5kg prepares, open and mix 30min, add again 0.6kg platinum complex compound, open with silane coupling agent (WD-60) 1kg of epoxy group(ing) and mix 30min and mix, vacuumize at last that (0.06MPa) 60min namely gets described single-component add-on type liquid silicon rubber;
The liquid silastic that makes is beaten in mould, be made into 50 * 50 * 6 under the 150 ℃/30min condition, the testing plate of 150 * 150 * 2mm, testing plate is placed 200 ℃ baking box again, post cure was carried out physical property measurement in 1 hour, and test result is shown in Table 1.
The physical property measurement result of the prepared liquid silastic of table 1
Shown by test result, the prepared liquid silastic of the present embodiment up to 5.5MPa, satisfies the bonding needs to stainless steel substrate to the stainless steel substrates bonding strength fully; Can deposit more than 90 days at normal temperature under the air-tight state.
Embodiment 2
A, prepare basic glue
1. adding 140kg viscosity in the 500L kneader is that 1000cp (25 ℃), contents of ethylene are the polysiloxane I of 1.2mol.%, and the aerosil of 100kg 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 1 hour;
3. being evacuated to vacuum tightness is 0.8MPa, under vacuum condition, continue to mediate 3 hours in 150～160 ℃, then stop to vacuumize, be cooled to 120 ℃, the polysiloxane I and the 36kg viscosity that add 80kg viscosity and be 1000cp (25 ℃), contents of ethylene and be 1.2mol.% are that 10000cp (25 ℃), contents of ethylene are the polysiloxane II of 5.0mol.%, mix, namely get described basic glue;
B, preparation single component glue
In the 300L planetary mixer, add the basic glue of the above-mentioned preparation of 200kg, hydrogen containing siloxane and the 0.08kg alkynol class inhibitor that 6.2kg prepares, open and mix 30min, add again 0.6kg platinum complex compound, titanate coupling agent, be that the mixture 1.5kg of 1:10 opens and mixes 30min and mix with the silane coupling agent mass ratio of the rare base of second, vacuumize at last that (0.06MPa) 60min namely gets described single-component add-on type liquid silicon rubber;
The liquid silastic that makes is beaten in mould, be made into 50 * 50 * 6 under the 150 ℃/30min condition, the testing plate of 150 * 150 * 2mm, testing plate is placed 200 ℃ baking box again, post cure was carried out physical property measurement in 1 hour, and test result is shown in Table 2.
The physical property measurement result of the prepared liquid silastic of table 2
Shown by test result, the prepared liquid silastic of the present embodiment up to 4.5MPa, satisfies the bonding needs to polyester material base material to polyester material bonding strength fully; Can deposit more than 90 days at normal temperature under the air-tight state.
Embodiment 3
A, prepare basic glue
1. the polysiloxane I, the 40kg viscosity that add 120kg viscosity and be 500cp (25 ℃), contents of ethylene in the 500L kneader and be 0.5mol.% are that 8000cp (25 ℃), contents of ethylene are the polysiloxane II of 2.5mol.%, the precipitated silica of 140kg 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 1 hour;
3. being evacuated to vacuum tightness is 0.8MPa, under vacuum condition, continue to mediate 3 hours in 150～160 ℃, then stop to vacuumize, be cooled to 120 ℃, adding 120kg viscosity is that 500cp (25 ℃), contents of ethylene are the polysiloxane I of 0.5mol.%, mix, namely get described basic glue;
B, preparation single component glue
In the 300L planetary mixer, add the basic glue of the above-mentioned preparation of 200kg, hydrogen containing siloxane and the 0.08kg alkynol class inhibitor that 2kg prepares, open and mix 30min, add again 0.3kg platinum complex compound, cerous oxide 4kg, open and mix 30min and mix, vacuumize at last that (0.06MPa) 60min namely gets described single-component add-on type liquid silicon rubber;
With the liquid silastic that makes, make testing plate through 300 ℃/168hr, test result is as follows:
Make tensile test after the curing, test result shows, the prepared liquid silastic of the present embodiment, and behind 300 ℃/168hr burn-in test, the tensile strength decay only has 40%, demonstrates good heat aging property, is applicable to the adhering and sealing of hot metal parts.
Embodiment 4
A, prepare basic glue
1. adding 220kg viscosity in the 500L kneader is that 5000cp (25 ℃), contents of ethylene are the polysiloxane I of 1.5mol.%, and the aerosil of 160kg 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 1 hour;
3. being evacuated to vacuum tightness is 0.8MPa, under vacuum condition, continue to mediate 3 hours in 150～160 ℃, then stop to vacuumize, be cooled to 120 ℃, adding 40kg viscosity is that 9000cp (25 ℃), contents of ethylene are the polysiloxane II of 3.5mol.%, mix, namely get described basic glue;
B, preparation single component glue
In the 300L planetary mixer, add the basic glue of the above-mentioned preparation of 200kg, hydrogen containing siloxane and the 0.4kg alkynol class inhibitor that 20kg prepares, open and mix 30min, add again 1kg platinum complex compound, titanate coupling agent 1.5kg, nanometer polytetrafluoroethylcomposite powder 2kg opens and mixes 30min and mix, and vacuumizes at last that (0.06MPa) 60min namely gets described single-component add-on type liquid silicon rubber;
The liquid silastic that this example makes as the oil seal of motor car engine, embodies better oil resistant and ageing resistance.
Claims (7)
1. a single-component add-on type liquid silicon rubber is characterized in that, consists of according to the mass fraction:
The composition of described basic glue, by mass percentage:
Polysiloxane I 30～70%
Polysiloxane II 4～30%
Water drain silica 20～40%;
Wherein, described polysiloxane I is that the viscosity 25 ℃ of mensuration is that 500～5000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 0.5～1.5mol.%; Described polysiloxane II is that the viscosity 25 ℃ of mensuration is that 8000～10000cp, contents of ethylene are the organopolysiloxane of the ethenyl blocking of 2.5～5.0mol.%; The composition general formula of the organopolysiloxane of described ethenyl blocking is: R
2SiO (SiRR ' O) nSiR
2, wherein R is vinyl, R ' is vinyl or methyl.
2. single-component add-on type liquid silicon rubber according to claim 1 is characterized in that, described platinum complex compound is synthetic by Platinic chloride and Virahol coordination, and platinum content wherein is 500～3000ppm.
3. single-component add-on type liquid silicon rubber according to claim 1, it is characterized in that, described hydrogen containing siloxane is to be 0.1-0.25mol.% by hydrogen content, viscosity is that end hydrogen based polysiloxane and the hydrogen content of 20-50 centipoise is 0.5-0.75mol.%, and viscosity is that the side group hydrogen containing siloxane of 20-50 centipoise forms for the ratio cooperation of 3-9:1 in mass ratio.
4. single-component add-on type liquid silicon rubber according to claim 1 is characterized in that, described alkynol class inhibitor is that encircling pure by heptamethylcyclotetrasiloxane and ethynyl-1-is 1-2:1 composite modified forming under the Platinic chloride effect by the mole mass ratio.
5. single-component add-on type liquid silicon rubber according to claim 1, it is characterized in that, described property-modifying additive comprise in the concentrated dispersion liquid of cerous oxide, zirconium dioxide, ferric oxide, nanometer polytetrafluoroethylcomposite powder, tetrafluoroethylene, silane coupling agent, titanate coupling agent, the aluminate coupling agent any one or multiple.
6. single-component add-on type liquid silicon rubber according to claim 1 is characterized in that, described water drain silica is aerosil or the precipitated silica after silane coupling agent is done the hydrophobic processing.
7. the preparation method of single-component add-on type liquid silicon rubber claimed in claim 1 is characterized in that, comprises the steps:
A, prepare basic glue:
1. the polysiloxane I of 50～100% formula ratios, the water drain silica of formula ratio are added in the kneader, at room temperature mediated 2～4 hours;
2. be warming up to 150～160 ℃, then constant temperature was mediated 1～2 hour;
3. vacuumize, under vacuum condition, continue to mediate 2～4 hours in 150～160 ℃, then stop to vacuumize, be cooled to 110～130 ℃, add the polysiloxane I of remaining formula ratio and the polysiloxane II of formula ratio, mix, namely get described basic glue;
Hydrogen containing siloxane, the alkynol class inhibitor of b, basic glue 100 mass parts of getting above-mentioned preparation, adding formula ratio stir, the platinum complex compound, the property-modifying additive that add formula ratio mix again, and vacuumize and namely get described single-component add-on type liquid silicon rubber.
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Application publication date: 20130918 |