CN110499032A - A kind of self-lubricating add-on type liquid silicon rubber and its preparation method and application - Google Patents
A kind of self-lubricating add-on type liquid silicon rubber and its preparation method and application Download PDFInfo
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- CN110499032A CN110499032A CN201910800917.2A CN201910800917A CN110499032A CN 110499032 A CN110499032 A CN 110499032A CN 201910800917 A CN201910800917 A CN 201910800917A CN 110499032 A CN110499032 A CN 110499032A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to a kind of self-lubricating add-on type liquid silicon rubber, the liquid silastic includes the raw material of following parts by weight: 120-200 parts of polysiloxanes containing alkenyl；1-15 parts of hydride silicones；30-80 parts of gas-phase silicas；10-30 parts of silazane white carbon black inorganic agents；1-30 parts of methyl phenyl silicone oils；0.004-0.06 parts of Si-H addition catalysts；0.03-0.6 parts of inhibitor.The present invention passes through the type and dosage of polysiloxanes containing alkenyl and hydride silicone in screening base rubber, component A and component B, the present invention controls permeability rate and properties of product by raw material screening, formula design, to provide a kind of add-on type liquid silicon rubber for having both high tearing toughness (>=45kN/m) and low permanent compression set rate (≤20%), permeability is stablized simultaneously, is able to maintain permanent self-lubricating effect.Self-lubricating add-on type liquid silicon rubber provided by the invention, preparation method is simple, and raw material is cheap and easy to get, is suitble to industrialized production.
Description
Technical field
The present invention relates to silicon rubber technical fields, and in particular to a kind of add-on type liquid silicon rubber.
Background technique:
Liquid silastic has good high and low temperature resistance, and performance change is small under wide temperature range, resistance to ozone, weatherability, electricity
Many excellent performances such as insulating properties, flame retardant property, while automation technolo degree height, high production efficiency, environmentally friendly no coupling product,
Application field is constantly expanded.But liquid silastic feature is that coefficient of friction is big, is worn no resistance, and limits it some
Low friction requires field application.
For self-lubricating silastic material after curing molding, product surface, which will be slow, is precipitated many tiny oil droplets.In this way may be used
Skin-friction force is effectively reduced, play the role of lubrication, it is possible to reduce or avoid the damage of product.Self-lubricating silicon rubber can be with
It is widely used in the fields such as electronics, automobile, medical treatment, such as core of a cable sealing, plugging member, O-ring, gasket, medical diaphragm
Deng.Self-lubricating liquid silastic, which will have, fuel-displaced continues controllable, good mechanical property and lower compressive deformation, to guarantee
The sealing of product and the requirement of service life.
Chinese patent CN104910633A discloses a kind of preparation method from permeability firm silicone rubber.Chinese patent
CN104479365B discloses a kind of preparation method from condensate oil firm silicone rubber, without referring to important index compressed shape
Become.Chinese patent CN106221240 discloses a kind of self-lubricating silicon rubber and preparation method thereof, and the silicon rubber tearing strength of preparation is low
(≤20KN/m) and preparation process complexity, it is not able to satisfy actual demand.There are some defects in above-mentioned patent: first, it needs to add
Preferable self-lubricating effect could be obtained by adding the phenyl silicone oil of higher proportion.Although certain infiltration can be played using phenyl silicone oil
Oily, fuel-displaced effect but fuel-displaced effect is deteriorated after long-time, cannot be persistently fuel-displaced, shorten the service life of silicon rubber；The
Two, firm silicone rubber base-material viscosity is high and the lower permeability agent phenyl silicone oil compatibility of viscosity is poor, is easy on a mill viscous
Rod, processing technology is complicated and has certain risk；If platinum catalyst is applied alone in third, from the compression of permeability solid silicone
Permanent set is up to 42%；Using double vulcanization platinum-peroxide vulcanizing systems, after post-cure, compressed shape variability is reduced
To 20%, but peroxide vulcanizing agent has peculiar smell, not environmentally friendly enough.Therefore, it needs exploitation one kind and has both low compression set
The self-lubricating add-on type liquid silicon rubber of rate and high tear strength.
Summary of the invention
In view of this, being designed the object of the present invention is to provide a kind of self-lubricating liquid silastic by raw material and formula
Mainly solve three key problems: 1. high tearing strengths (>=45KN/m) meet the anti-tear demand installed and used；2. platinum sulphur
Change liquid glue have ultralow Compression Set (be not necessarily to post-cure, the primary compression set rate that vulcanizes lower than 20%),
The leakproofness for improving material, meets end products durability requirements；3. long-term controllable lubricity, meets self-lubricating and high life
Demand.
A kind of self-lubricating add-on type liquid silicon rubber, the raw material including following parts by weight: the 120-200 parts of poly- silicon oxygen containing alkenyl
Alkane；1-15 parts of hydride silicones；30-80 parts of gas-phase silicas；10-30 parts of silazane white carbon black inorganic agents；1-30 parts of methyl
Phenyl silicone oil；0.004-0.06 parts of Si-H addition catalysts；0.03-0.6 parts of inhibitor.
Preferably, the self-lubricating add-on type liquid silicon rubber is two-component, including component A and component B, wherein component A
Raw material including following parts by weight: 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils,
0.005-0.06 parts of Si-H addition catalysts；Component B includes the raw material of following parts by weight: 100-130 parts of base rubbers, 0-30 parts contain alkene
Based polysiloxane, 0-15 part methyl phenyl silicone oil, 0.03-0.6 parts of inhibitor, 1-15 parts of hydride silicones；The 100-130
Part base rubber is by including 60-80 parts of polysiloxanes containing alkenyl, 15-40 parts of gas-phase silicas, 5-15 parts of silazane white carbon blacks processing
Agent is made；
Condition is component A and the total dosage of B component methyl phenyl silicone oil is 1-30 parts.
It is further preferred that the self-lubricating add-on type liquid silicon rubber is two-component, including component A and component B, wherein
Component A includes the raw material of following parts by weight: 100-130 parts of base rubbers, 5-20 parts of polysiloxanes containing alkenyl, 1-5 parts of aminomethyl phenyl silicon
Oil, 0.005-0.02 parts of Si-H addition catalysts；Component B includes the raw material of following parts by weight: 100-130 parts of base rubbers, 5-20 parts
Polysiloxanes containing alkenyl, 1-5 part methyl phenyl silicone oil, 0.05-0.4 parts of inhibitor, 4-10 parts of hydride silicones；The base rubber
By being made including 60-80 parts of polysiloxanes containing alkenyl, 20-30 parts of gas-phase silicas, 5-15 parts of silazane white carbon black inorganic agents.
As known in those skilled in the art, when having alkenyl polysiloxanes and hydride silicone in component,
A certain amount of inhibitor, which is added, inhibits it instead to give birth to Si-H addition reaction.
In the present invention, polysiloxanes containing alkenyl is the polysiloxanes of the alkenyl containing carbon-carbon double bond, and the alkenyl is ethylene
At least one of base, acrylic, cyclobutenyl, on the end group and/or side chain of polysiloxanes, amount vinyl content is the alkenyl
0.02-1mmol/g；Hydride silicone refers to the end group that reactive hydrogen mass content is 2-16mmol/g and/or side chain containing activity
The polysiloxanes of hydrogen；
Preferably, the amount vinyl content of the component A and/or the polysiloxanes containing alkenyl in component B is 0.03-
The alkenyl polysiloxanes of 0.9mmol/g；The reactive hydrogen mass content of hydride silicone is 2-12mmol/g.
It is further preferred that alkenyl viscosity of polysiloxane of the end group in component A and component B containing alkenyl is 3500-
30000mPas amount vinyl content is 0.02-0.25mmol/g, and more preferable viscosity is 10000-30000mPas, and amount vinyl content is
0.03-0.1mmol/g；Alkenyl viscosity of polysiloxane of the side chain containing alkenyl is 1000-5000mPas, amount vinyl content 0.1-
0.3mmol/g, more preferable viscosity are that 1000-2000mPas amount vinyl content is 0.1-0.2mmol/g；End group and side chain contain alkene
The alkenyl viscosity of polysiloxane of base is 300-1000mPas, amount vinyl content 0.6-1mmol/g, more preferable viscosity 400-
The content of 700mPas alkenyl is 0.7-0.9mmol/g；
And/or the active hydrogen content of the end group hydrogen containing siloxane is 2-5mmol/g, the work of side chain hydrogen containing siloxane
Property hydrogen content be 2.5-15mmol/g, the active hydrogen content of end group and the equal hydrogen containing siloxane of side chain is 3-15mmol/g.
More preferably, the alkenyl polysiloxanes includes the polysiloxanes that side chain must contain alkenyl, i.e., the described poly- silicon of alkenyl
Oxygen alkane includes the combination of one or both of the polysiloxanes of side chain alkenyl polysiloxanes and end group and side chain containing alkenyl, item
Part is that side chain alkenyl polysiloxanes and end group and the side chain total dosage of the polysiloxanes containing alkenyl are 2- in component A and B component
20 parts, preferably 10-20 parts.
In the present invention, the preparation method of the base rubber is the following steps are included: be 60000mPas- by 40-45 parts of viscosity
1000000mPas, amount vinyl content are the end group polysiloxanes containing alkenyl of 0.02-0.035mmol/g, and 2-5 parts of viscosity are
The side chain polysiloxanes containing alkenyl of 100000mPas-250000mPas, amount vinyl content 0.6-1.0mmol/g, 15-40 parts of gas
Phase white carbon black and 5-15 parts of silazane are uniformly mixed in water, and it is small to be sufficiently mixed 1-2 under 60-90 DEG C or less inert atmosphere protection
When, start to vacuumize 2-4h after being then warming up to 130-180 DEG C, 130-180 DEG C is maintained the temperature at when vacuumizing, is then cooled to
120-140 DEG C, adding 15-20 parts of viscosity is 20000mPas-60000mPas, amount vinyl content 0.03-0.07mmol/g
End group polysiloxanes containing alkenyl be diluted, stir evenly to get to base rubber.
It is that single phenyl seals that the methyl phenyl silicone oil, which is selected from both ends with double phenyl end capped methyl phenyl silicones, both ends,
Any one or more mixing in the methyl phenyl silicone at end, the methyl phenyl silicone that both ends are methyl blocking, preferably
The double phenyl end capped methyl phenyl silicones in both ends；The methyl phenyl silicone oil is the first of one or more different indexs of refraction
The mixture of base phenyl silicone oil, range of viscosities 50-500mpas, preferably 100-300mpas.
There is no particular limitation for the inhibitor, and this field can inhibit the reagent of Si-H addition, generally alkynol
Substance, adducible example include but is not limited to 1- acetenyl -1- cyclohexanol, 2- methyl -3- butine -ol and 3,5- diformazan
At least one of the pure and mild 3- methyl-1 of base -1- hexin -3--dodecyne -3- alcohol.
The Si-H addition catalyst is transition metal oxides and its complex compound such as Karst type, Cabbeen type, support type,
It is preferred that Karst type platinum catalyst.
The white carbon black is the gas-phase silica handled by the situ-formed graft of the inorganic agents such as silazane, and specific surface area is not
Less than 200m2/ g, preferably 250-400m2/g；The white carbon black inorganic agent is hexa methyl silazane, tetramethyl divinyl silicon
Azane, heptamethyldisilazane, vinyl double seal head, at least one of hydroxy silicon oil.
The present invention also provides the preparation methods of the self-lubricating add-on type liquid silicon rubber, comprising the following steps:
(1) preparation of base rubber: by including 60-80 parts of polysiloxanes containing alkenyl, 15-40 parts of gas-phase silicas, 5-15 parts of silicon
The raw material of azane white carbon black inorganic agent, is made under 130-180 DEG C of vacuum condition；
(2) component A prepare: by 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils,
0.005-0.06 parts of Si-H addition catalysts mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silastic A group
Point；
(3) B component prepare: by 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils,
0.03-0.6 parts of inhibitor, 1-15 parts of hydride silicones mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silicon
Rubber B component；
Condition is that the dosage that methyl phenyl silicone oil is total in component A and B component is 1-30 parts.
Preferably, the preparation method of the self-lubricating add-on type liquid silicon rubber, comprising the following steps:
(1) preparation of base rubber: by including 60-80 parts of polysiloxanes containing alkenyl, 20-30 parts of gas-phase silicas, 5-15 parts of silicon
The raw material of azane white carbon black inorganic agent, is made under 130-180 DEG C of vacuum condition；
(2) component A prepare: by 100-130 parts of base rubbers, 5-20 parts of polysiloxanes containing alkenyl, 1-5 parts of methyl phenyl silicone oils,
0.005-0.02 parts of Si-H addition catalysts mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silastic A group
Point；
(3) B component prepare: by 100-130 parts of base rubbers, 5-20 parts of polysiloxanes containing alkenyl, 1-5 parts of methyl phenyl silicone oils,
0.03-0.4 parts of inhibitor, 4-10 parts of hydride silicones mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silicon
Rubber B component；
It is known in those skilled in the art to be, when containing alkenyl polysiloxanes and hydride silicone in component,
The reaction that inhibitor inhibits between the two should be added in component.
The present invention also provides the purposes of the self-lubricating add-on type liquid silicon rubber, answer for electronics, automobile, medical treatment
Use field.Tearing strength >=45KN/m of the self-lubricating add-on type liquid silicon rubber, primary vulcanization compression set rate are low
In 20%.
The process conditions such as temperature of the present invention, time are preferred scope, but protection scope of the present invention is not limited to
This.
Compared with prior art, the invention has the following advantages:
One, to the Nomenclature Composition and Structure of Complexes of polysiloxanes containing alkenyl and hydride silicone in liquid silastic bi-component, than
If proportion and alkenyl, the content of reactive hydrogen of its raw material are specifically selected, cooperates other raw materials to obtain and have both highly resistance
Tear the liquid silastic of intensity and ultralow platinum vulcanization compression set rate.
Two, the self-lubricating liquid silastic of high tear strength is obtained, product tear strength is higher than 42KN.m-1, it is much higher than
The 15-30KN.m of patent report at present-1。
Three, it is lower than 20% obtained from the primary vulcanization compression set rate of lubrication product, the country has not been reported.
Four, by the regulation to product crosslink density, phenyl silicone oil type and additive amount, product permeability rate and length are realized
The control of phase lubrication.
Specific embodiment
Self-lubricating add-on type liquid silicon rubber of the invention is described further combined with specific embodiments below, but this hair
It is bright to be not limited to following embodiment.Unless otherwise defined, all technical terms used hereinafter and those skilled in the art
Normally understood meaning is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not
It is intended to limit the scope of the invention.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Term described in specific embodiment " part " refers both to parts by weight if without specified otherwise.
Preparation exampleThe preparation of base rubber
Preparation example 1
It is 42 parts of viscosity by weight accounting in kneader or planetary mixer is 60000mPas, the content of alkenyl
For the end-vinyl polysiloxanes of 0.03mmol/g, 2.8 parts of viscosity 200000mPas, the content of alkenyl is 0.8mmol/g's
Pendant vinyl based polysiloxane, 25 parts of BET specific surface areas are 300m2The gas-phase silica of/g and 7.05 parts of two silicon of hexamethyl
Azane, 0.15 part of tetramethyl divinyl silazane and 6.5 parts of deionized water are filled under 80 DEG C or less inert atmosphere protections
Point mixing 1~2 hour, start to vacuumize 2~4h after being then warming up to 130~150 DEG C, maintain the temperature at 150 when vacuumizing~
170 DEG C, 110~140 DEG C are then cooled to, 16.5 parts of viscosity 20000mPas are added, the content of vinyl is 0.035mmol/
The end g alkenyl polysiloxanes stirs evenly to get liquid silastic base rubber 1 is arrived.
Preparation example 2
It is 40 parts of viscosity by weight accounting in kneader or planetary mixer is 60000mPas, the content of alkenyl
Methylvinyl-polysiloxane, 3 parts of viscosity for 0.03mmol/g are 250000mPas, and the content of alkenyl is 0.9mmol/g
More vinyl polysiloxanes, 27.5 parts of BET specific surface areas be 400m2The gas-phase silica of/g and 8 parts of two silicon of hexamethyl
Azane, 0.5 part of tetramethyl divinyl silazane and 4.5 parts of deionized water are filled under 80 DEG C or less inert atmosphere protections
Point mixing 1~2 hour, start to vacuumize 2~4h after being then warming up to 130~150 DEG C, maintain the temperature at 150 when vacuumizing~
170 DEG C, 110~140 DEG C are then cooled to, it is 60000mPas that 17 parts of viscosity, which are added, and the content of alkenyl is 0.030mmol/g
Methylvinyl-polysiloxane stirs evenly to get liquid silastic base rubber 2 is arrived.
Compare preparation example 1
It is 60 parts of viscosity by weight accounting in kneader or planetary mixer is 60000mPas, vinyl contains
Amount is the end-vinyl polysiloxanes of 0.035mmol/g, and 25 parts of BET specific surface areas are 300m2The gas-phase silica of/g and
7.05 parts of hexamethyldisilazane, 0.15 part of tetramethyl divinyl silazane and 6.5 parts of deionized water, 80 DEG C with
It is sufficiently mixed under lower inert atmosphere protection 1~2 hour, starts to vacuumize after being then warming up to 130~150 DEG C, guarantor when vacuumizing
Temperature is held at 150~170 DEG C, then cools to 110~140 DEG C, is stirred evenly to get liquid silastic base rubber 3 is arrived.
EmbodimentThe preparation of liquid silastic
Embodiment 1
The preparation of AB component: being 20000mPas by above-mentioned 100 parts .1 parts of viscosity of base rubber Isosorbide-5-Nitrae, and amount vinyl content is
The terminal ethylenic based polysiloxane of 0.035mmol/g, 7.2 parts of viscosity are 1000mPas, and part amount vinyl content is 0.12mmol/g
Pendant vinyl based polysiloxane, 3.0 parts of viscosity are 400mPas, and amount vinyl content is that the end group of 0.9mmol/g and side chain contain
The polysiloxanes of vinyl, 0.014 part of Karst catalyst, 2.3 parts of viscosity are 300mPas methyl phenyl silicone oil, in planet
It is dispersed with stirring 30-40min in blender, is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid silastic A group
Point.It is 20000mPas by 1,8.8 parts of viscosity of above-mentioned 100 parts of base rubber, amount vinyl content is the terminal ethylenic of 0.035mmol/g
Based polysiloxane vinyl polysiloxane, 3.5 parts of viscosity are 400mPas, and amount vinyl content is the end group and side chain of 0.9mmol/g
Containing the polysiloxanes of vinyl, 2.3 parts of viscosity are 200mPas methyl phenyl silicone oil mixture, and 5.1 parts of quality hydrogen contents are
7mmol/g side chain contains the hydride silicone of Si-H, and 0.08 part of 3- methyl-1-dodecyne-3- alcohol stirs in planetary mixer
Dispersion 30-40min is mixed, vacuumizing and defoaming is uniformly mixed again and obtains self-lubricating low pressure change liquid silastic B component.
Embodiment 1-1
According to the identical method preparation of liquid silicone rubber of embodiment 1, when difference is to prepare component A, viscosity is
1000mPas, the pendant vinyl based polysiloxane dosage that amount vinyl content is 0.12mmol/g is 15 parts.
Embodiment 1-2
According to the identical method preparation of liquid silicone rubber of embodiment 1, when difference is to prepare component A, viscosity is
1000mPas, the pendant vinyl based polysiloxane dosage that amount vinyl content is 0.12mmol/g is 2 parts.
Embodiment 2
The preparation of AB component: being 20000mPas by 2,6.1 parts of viscosity of above-mentioned 120 parts of base rubber, and amount vinyl content is
The end-vinyl polysiloxanes of 0.035mmol/g, 5.2 parts of viscosity are 1000mPas, and the content of alkenyl is 0.12mmol/g
Pendant vinyl based polysiloxane, 3.5 parts of viscosity are 100mPas methyl phenyl silicone oil mixture, 0.015 part of Karst catalysis
Agent is dispersed with stirring 30-40min in planetary mixer, is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid
Silicon rubber component A.It is 400mPas by 1,5.5 parts of viscosity of above-mentioned 120 parts of base rubber, amount vinyl content is the end group of 0.9mmol/g
Contain vinyl polysiloxane with side chain, the hydride silicone that the side chain that 2.3 parts of hydrogen contents are 7mmol/g contains Si-H, 0.9
For the end group and side chain that part hydrogen content is 13mmol/g containing the hydride silicone of SiH, 3 parts of viscosity are 100mPas methyl
Phenyl silicone oil mixture, 0.09 part of 1- acetenyl -1- cyclohexanol are dispersed with stirring 30-40min in planetary mixer, and mixing is equal
Even vacuumizing and defoaming again obtains self-lubricating low pressure and becomes liquid silastic B component.
Embodiment 3
The preparation of AB component: being 24000mPas by 1,9.2 parts of viscosity of above-mentioned 100 parts of base rubber, and amount vinyl content is
The terminal ethylenic based polysiloxane of 0.042mmol/g, 2.1 parts of viscosity are 1000mPas, and amount vinyl content is 0.12mmol/g's
Pendant vinyl based polysiloxane, 1.2 parts of viscosity are 400mPas, and amount vinyl content is that the end group of 0.9mmol/g and side chain contain second
Alkenyl polysiloxanes, 0.014 part of Karst catalyst, 2.3 parts of viscosity are 300mPas methyl phenyl silicone oil, in planet stirring
It is dispersed with stirring 30-40min in machine, is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid silastic component A.It will
1,2.1 parts of viscosity of above-mentioned 100 parts of base rubber are 1000mPas, and amount vinyl content is the poly- silicon oxygen of ethenyl of side chain of 0.12mmol/g
Alkane, 5.5 parts of viscosity are 400mPas, and amount vinyl content is the end group of 0.9mmol/g and side chain contains vinyl polysiloxane, 2.3
Part viscosity is 200mPas methyl phenyl silicone oil mixture, and 4.5 parts of hydrogen contents are that the end group of 10mmol/g and side chain contain
The hydride silicone of Si-H, 0.08 part of 3- methyl-1-dodecyne-3- alcohol, is dispersed with stirring 30-40min in planetary mixer,
It is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid silastic B component.
Embodiment 4
The preparation of AB component: being 20000mPas, amount vinyl content 0.035mmol/ by 100 parts .7 parts of viscosity of base rubber Isosorbide-5-Nitrae
The terminal ethylenic based polysiloxane of g, 2.6 parts of viscosity are 1000mPas, and amount vinyl content is the ethenyl of side chain of 0.12mmol/g
Polysiloxanes, 1.2 parts of viscosity are 400mPas, and amount vinyl content is 0.9mmol/g end group and the side chain poly- silicon oxygen containing vinyl
Alkane, 0.014 part of Karst catalyst, 0.08 part of 3- methyl-1-dodecyne-3- alcohol, 2.3 parts of viscosity are 300mPas methylbenzene
Base silicone oil, is dispersed with stirring 30-40min in planetary mixer, is uniformly mixed again vacuumizing and defoaming and obtains the change of self-lubricating low pressure
Liquid silastic component A.It is 20000mPas by 1,5.3 parts of viscosity of above-mentioned 100 parts of base rubber, amount vinyl content is
The terminal ethylenic based polysiloxane of 0.035mmol/g, 4.8 parts of viscosity are 1000mPas, and amount vinyl content is 0.12mmol/g's
Pendant vinyl based polysiloxane, 5.5 parts of viscosity are 400mPas, and amount vinyl content is that the end group of 0.9mmol/g and side chain contain second
The polysiloxanes of alkenyl, 2.3 parts of viscosity are 200mPas methyl phenyl silicone oil mixture, and 2.5 parts of hydrogen contents are the side 7mmol/g
It is poly- that chain contains the hydride silicone of Si-H, the end group that 3.1 parts of hydrogen contents are 10mmol/g and the side chain hydrogenation containing Si-H
Siloxanes is dispersed with stirring 30-40min in planetary mixer, is uniformly mixed again vacuumizing and defoaming and obtains the change of self-lubricating low pressure
Liquid silastic B component.
Embodiment 5
The preparation of AB component: being 20000mPas, amount vinyl content 0.035mmol/g by 100 parts 1,5 parts of viscosity of base rubber
Terminal ethylenic based polysiloxane, 3.6 parts of viscosity are 1000mPas, and the ethenyl of side chain that amount vinyl content is 0.12mmol/g is poly-
Siloxanes, 3.3 parts of viscosity are 400mPas, and amount vinyl content is 0.9mmol/g end group and the side chain poly- silicon oxygen containing vinyl
Alkane, 0.018 part of Karst catalyst, 0.06 part of 3- methyl-1-dodecyne-3- alcohol, 2.3 parts of viscosity are 300mPas methylbenzene
The mixing of base silicone oil, is dispersed with stirring 30-40min in planetary mixer, and it is low that uniformly mixed vacuumizing and defoaming again obtains self-lubricating
Buckling liquid silastic component A.It is 20000mPas, amount vinyl content 0.035mmol/g by 100 parts 1,5 parts of viscosity of base rubber
Terminal ethylenic based polysiloxane, 3.6 parts of viscosity are 1000mPas, and the ethenyl of side chain that amount vinyl content is 0.12mmol/g is poly-
Siloxanes, 3.3 parts of viscosity are 400mPas, and amount vinyl content is 0.9mmol/g end group and the side chain poly- silicon oxygen containing vinyl
Alkane, the end group and side chain that 4.5 parts of hydrogen contents are 10mmol/g are containing the hydride silicone of Si-H, 0.06 part of 3- methyl-1-
Dodecyne -3- alcohol, 2.3 parts of viscosity are the mixing of 300mPas methyl phenyl silicone oil, and 30- is dispersed with stirring in planetary mixer
40min is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid silastic B component.
Embodiment 6
The preparation of AB component: being 20000mPas, amount vinyl content 0.035mmol/ by 100 parts 2,4.7 parts of viscosity of base rubber
The terminal ethylenic based polysiloxane of g, 4.2 parts of viscosity are 1000mPas, and amount vinyl content is the ethenyl of side chain of 0.12mmol/g
Polysiloxanes, 2.4 parts of viscosity are 400mPas, and amount vinyl content is 0.9mmol/g end group and the side chain poly- silicon oxygen containing vinyl
Alkane, 0.018 part of Karst catalyst, 0.06 part of 3- methyl-1-dodecyne-3- alcohol, 2.3 parts of viscosity are 300mPas methylbenzene
The mixing of base silicone oil, is dispersed with stirring 30-40min in planetary mixer, and it is low that uniformly mixed vacuumizing and defoaming again obtains self-lubricating
Buckling liquid silastic component A.It is 20000mPas by 100 parts 2,5.1 parts of viscosity of base rubber, amount vinyl content is
The terminal ethylenic based polysiloxane of 0.035mmol/g, 2.3 parts of viscosity are 1000mPas, and amount vinyl content is 0.12mmol/g's
Pendant vinyl based polysiloxane, 4.7 parts of viscosity are 400mPas, and amount vinyl content is that 0.9mmol/g end group and side chain contain ethylene
The polysiloxanes of base, the end group and side chain that 4.5 parts of hydrogen contents are 10mmol/g are containing the hydride silicone of Si-H, and 0.06 part
3- methyl-1-dodecyne-3- alcohol, 2.3 parts of viscosity are the mixing of 300mPas methyl phenyl silicone oil, are stirred in planetary mixer
Disperse 30-40min, is uniformly mixed again vacuumizing and defoaming and obtains self-lubricating low pressure change liquid silastic B component.
Comparative example 1
Other steps are same as Example 1, and difference is the base rubber 3 using comparison preparation example 1.
Comparative example 2
Other steps are same as Example 1, when difference is to prepare component A and B component, are added without the poly- silicon of ethenyl of side chain
Oxygen alkane.
Application examples
The detection method of compression set uses GB/T 7759；The detection method of tensile strength and elongation at break is adopted
With ASTM D412；The detection method of hardness uses ASTM D2240；The detection method of tearing strength uses ASTM D624；Rebound
The detection method of rate uses ASTM D7121；Permeability speed detection method is the quality amount of precipitation for testing phenyl silicone oil.
Tensile strength, elongation at break, hardness, tearing strength, the test sample of rebound degree and condensate oil rate are will to implement
After component A and B component in example are mixed according to the allotment of 1:1 ratio, solidifies 5min at 170 DEG C and 2mm test piece is made.Calculate compression
Set deformation volume DRC is that diameter 29.5mm is made according to national standard, height h0The test block of (12.5mm or so), then with suitable
Limiter height h2Test block is compressed 25%, is placed in aging 22h in 180 DEG C of baking ovens, the constant temperature under 25 DEG C of 50% humidity
The thickness h of cooling half an hour test test block1, according to formula DRC=(h0-h1)/(h0-h2) * 100%.
Properties of product in 1-7 of the embodiment of the present invention and comparative example 1 are compared, the results are shown in Table 1.
Table 1
Table 1 is that the performance of liquid silastic silica gel piece made from embodiment and comparative example compares.As known from Table 1, of the invention
The liquid silastic excellent combination property of offer especially has very high tearing toughness (>=45kN/m) and low permanent pressure
Compression deformation rate (≤20%).Liquid silastic self-lubricating property provided by the invention is good, and permeability amount is stablized, 30 days permeabilitys
Amount is also able to satisfy need satisfaction actual demand.
Above content is merely a preferred embodiment of the present invention, and is not intended to limit embodiment of the present invention, and this field is general
Logical technical staff's central scope according to the present invention and spirit can very easily carry out corresponding flexible or modification, therefore
Protection scope of the present invention should be subject to protection scope required by claims.
Claims (10)
1. a kind of self-lubricating add-on type liquid silicon rubber, the raw material including following parts by weight: the 120-200 parts of poly- silicon oxygen containing alkenyl
Alkane；1-15 parts of hydride silicones；30-80 parts of gas-phase silicas；10-30 parts of silazane white carbon black inorganic agents；1-30 parts of methyl
Phenyl silicone oil；0.004-0.06 parts of Si-H addition catalysts；0.03-0.6 parts of inhibitor.
2. liquid silastic as described in claim 1, which is characterized in that including component A and component B, wherein component A includes such as
The raw material of lower parts by weight: 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils, 0.005-
0.06 part of Si-H addition catalyst；Component B includes the raw material of following parts by weight: 100-130 parts of base rubbers, the 0-30 parts of poly- silicon containing alkenyl
Oxygen alkane, 0-15 part methyl phenyl silicone oil, 0.03-0.6 parts of inhibitor, 1-15 parts of hydride silicones；The 100-130 parts of base rubber
By being made including 60-80 parts of polysiloxanes containing alkenyl, 15-40 parts of gas-phase silicas, 5-15 parts of silazane white carbon black inorganic agents；
Condition is component A and the total dosage of B component methyl phenyl silicone oil is 1-30 parts.
3. liquid silastic as claimed in claim 2, which is characterized in that the self-lubricating add-on type liquid silicon rubber is double groups
Part, including component A and component B, wherein component A includes the raw material of following parts by weight: 100-130 part base rubbers, 5-20 parts containing alkenyl
Polysiloxanes, 1-5 part methyl phenyl silicone oil, 0.005-0.02 parts of Si-H addition catalysts；Component B includes the original of following parts by weight
Material: 100-130 parts of base rubbers, 5-20 parts of polysiloxanes containing alkenyl, 1-5 parts of methyl phenyl silicone oils, 0.05-0.4 parts of inhibitor, 4-10
Part hydride silicone；The base rubber is by including 60-80 parts of polysiloxanes containing alkenyl, 20-30 parts of gas-phase silicas, 5-15 parts
Silazane white carbon black inorganic agent is made.
4. liquid silastic as described in claim 1, which is characterized in that polysiloxanes containing alkenyl is the alkene containing carbon-carbon double bond
The polysiloxanes of base, the alkenyl are at least one of vinyl, acrylic and cyclobutenyl, and the alkenyl is at the end of polysiloxanes
On base and/or side chain, amount vinyl content 0.02-1mmol/g；Hydride silicone refers to that reactive hydrogen molar content is 2-
The polysiloxanes of end group and/or side chain containing reactive hydrogen of 16mmol/g；
Preferably, the amount vinyl content of the component A and/or the polysiloxanes containing alkenyl in component B is 0.03-0.9mmol/g
Alkenyl polysiloxanes；The reactive hydrogen molar content of hydride silicone is 2-12mmol/g.
5. liquid silastic as claimed in claim 4, which is characterized in that alkenyl of the end group containing alkenyl in component A and component B
Viscosity of polysiloxane is that 3500-30000mPas amount vinyl content is 0.02-0.25mmol/g, and more preferable viscosity is 10000-
30000mPas, amount vinyl content 0.03-0.1mmol/g；Alkenyl viscosity of polysiloxane of the side chain containing alkenyl is 1000-
5000mPas, amount vinyl content 0.1-0.3mmol/g, more preferable viscosity are that 1000-2000mPas amount vinyl content is 0.1-
0.2mmol/g；End group and the side chain alkenyl viscosity of polysiloxane containing alkenyl are 300-1000mPas, amount vinyl content 0.6-
1mmol/g, the content of more preferable viscosity 400-700mPas alkenyl are 0.7-0.9mmol/g；
And/or the active hydrogen content of the end group hydrogen containing siloxane is 2-5mmol/g, the reactive hydrogen of side chain hydrogen containing siloxane
Content is 2.5-15mmol/g, and the active hydrogen content of end group and the equal hydrogen containing siloxane of side chain is 3-15mmol/g.
6. liquid silastic as claimed in claim 5, which is characterized in that the alkenyl polysiloxanes includes that side chain must contain alkenyl
Polysiloxanes, i.e., the described alkenyl polysiloxanes includes side chain alkenyl polysiloxanes and end group and the side chain poly- silicon oxygen containing alkenyl
The combination of one or both of alkane, condition are that side chain polysiloxanes containing alkenyl contains with end group and side chain in component A and B component
The total dosage of the polysiloxanes of alkenyl is 2-20 parts, preferably 10-20 parts.
7. liquid silastic as claimed in claim 2 or claim 3, which is characterized in that the preparation method of the base rubber includes following step
It is rapid: to be 60000mPas-1000000mPas by 40-45 parts of viscosity, amount vinyl content is the end group of 0.02-0.035mmol/g
Polysiloxanes containing alkenyl, 2-5 parts of viscosity are 100000mPas-250000mPas, the side of amount vinyl content 0.6-1.0mmol/g
Chain polysiloxanes containing alkenyl, 15-40 parts of gas-phase silicas and 5-15 parts of silazane are uniformly mixed in water, at 60-90 DEG C or less
It is sufficiently mixed under inert atmosphere protection 1-2 hours, starts to vacuumize 2-4h after being then warming up to 130-180 DEG C, guarantor when vacuumizing
Temperature is held at 130-180 DEG C, then cools to 120-140 DEG C, adding 15-20 parts of viscosity is 20000mPas-
The end group polysiloxanes containing alkenyl of 60000mPas, amount vinyl content 0.03-0.07mmol/g are diluted, stir evenly to get
To base rubber.
8. liquid silastic as described in any one of claims 1-3, which is characterized in that the methyl phenyl silicone oil is selected from both ends
With double phenyl end capped methyl phenyl silicones, both ends be single phenyl end capped methyl phenyl silicone, both ends are methyl
The double phenyl end capped poly- silicon oxygen of aminomethyl phenyl of any one or more mixing in the methyl phenyl silicone of sealing end, preferably both ends
Alkane；The range of viscosities of the methyl phenyl silicone oil is 50-500mpas, preferably 100-300mpas；And/or
The inhibitor is selected from 1- acetenyl -1- cyclohexanol, 2- methyl -3- butine -ol and 3,5- dimethyl -1- hexin -3- alcohol
At least one of with 3- methyl-1-dodecyne-3- alcohol；And/or
The Si-H addition catalyst is in the transition metal oxides such as Karst type, Cabbeen type, support type and its complex compound
At least one, preferred Karst type platinum catalyst；And/or
The white carbon black is the gas-phase silica handled by the situ-formed graft of inorganic agent, and specific surface area is no less than 200m2/ g,
Preferably 250-400m2/g；The white carbon black inorganic agent is hexa methyl silazane, tetramethyl divinyl silazane, seven methyl
Disilazane, vinyl double seal head, at least one of hydroxy silicon oil.
9. the preparation method of any one of the claim 1-8 liquid silastic, comprising the following steps:
(1) preparation of base rubber: by including 60-80 parts of polysiloxanes containing alkenyl, 15-40 parts of gas-phase silicas, 5-15 parts of silazane
The raw material of white carbon black inorganic agent is made under 130-180 DEG C of vacuum condition；
(2) component A prepare: by 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils,
0.005-0.06 parts of Si-H addition catalysts mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silastic A group
Point；
(3) B component prepare: by 100-130 parts of base rubbers, 0-30 parts of polysiloxanes containing alkenyl, 0-15 parts of methyl phenyl silicone oils,
0.03-0.6 parts of inhibitor, 1-15 parts of hydride silicones mix the vacuumizing and defoaming that is uniformly dispersed again and obtain self-lubricating liquid silicon
Rubber B component；
Condition is that the dosage that methyl phenyl silicone oil is total in component A and B component is 1-30 parts.
10. the purposes of the described in any item self-lubricating add-on type liquid silicon rubbers of claim 1-8, which is characterized in that for electricity
Son, automobile, medical application fields.
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