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CN104817845A - Liquid silicon rubber and preparation method thereof - Google Patents

Liquid silicon rubber and preparation method thereof Download PDF

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Publication number
CN104817845A
CN104817845A CN201510217623.9A CN201510217623A CN104817845A CN 104817845 A CN104817845 A CN 104817845A CN 201510217623 A CN201510217623 A CN 201510217623A CN 104817845 A CN104817845 A CN 104817845A
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linear poly
hydrogen siloxane
weight part
base
liquid silastic
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袁振乐
金子超
来立群
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Zhejiang Xinan Chemical Industrial Group Co Ltd
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Zhejiang Xinan Chemical Industrial Group Co Ltd
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Abstract

The invention belongs to the field of silicon rubber, and particularly relates to liquid silicon rubber and a preparation method thereof. The liquid silicon rubber is prepared by mixing, heating and curing the following materials in parts by weight in sequence: 100-300 parts of polysiloxane, 0.2-20 parts of linear hydropolysiloxane, 30-150 parts of white carbon black, 0.002-0.1 part of catalyst and 0.01-1 part of inhibitor, wherein the polysiloxane does not contain Si-H structure and at least two substituted groups are aliphatic unsaturated groups; the linear hydropolysiloxane comprises first linear hydropolysiloxane,; the first linear hydropolysiloxane is the linear hydropolysiloxane of which a chain end does not contain the Si-H structure and at least three side groups are hydrogen groups. The linear hydropolysiloxane of the special structure is added in the preparation process of the liquid silicon rubber, so that the prepared liquid silicon rubber has higher tensile strength and tear strength. Experiment results prove that the tensile strength of the provided liquid silicon rubber can reach up to 8.9 MPa and the tear strength can reach up to 50 KN/m, B.

Description

A kind of liquid silastic and preparation method thereof
Technical field
The invention belongs to silicone rubber art, particularly relate to a kind of liquid silastic and preparation method thereof.
Background technology
Now because liquid silastic has high-low temperature resistant, ultraviolet resistance, radiation hardness, the performance that weather-proof, electrical isolation, highly air-permeable, physiological inertia etc. are excellent, therefore obtain and apply widely in Aeronautics and Astronautics, electronic apparatus, chemical industry, machinery, medical science, daily necessities etc.
Liquid silastic is except meeting except the basic demand of medical macromolecular materials, also have heat-resisting, cold-resistant, nontoxic, resistance to biological aging, to minimum, the good physical and mechanical property holding point of the reaction of tissue, meets the requirement of medical macromolecular materials, become the most typical organosilicon macromolecule material in medical macromolecular materials, more and more wide in the application of medicine and hygiene fields.
Patent CN102827479A discloses a kind of preparation method of liquid silastic, the method adopts surface through the white carbon black of hexamethyldisilazane, silane coupling agent process as reinforced filling, obtained the liquid silastic of high-tear strength, but the tensile strength of this liquid silastic is lower; Patent CN103834177A also discloses a kind of preparation method of liquid silastic, and the pretreated white carbon black of same employing is as reinforced filling, and the tensile strength of the liquid silastic that the method obtains is higher, but tear strength is lower.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of liquid silastic and preparation method thereof, liquid silastic provided by the invention has higher tensile strength and tear strength.
The invention provides a kind of liquid silastic, by material successively through mixing, being heating and curing and making, with weight parts, described material comprises:
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
Preferably, described linear poly-hydrogen siloxane also comprises the second linear poly-hydrogen siloxane;
Described second linear poly-hydrogen siloxane is that side base is not hydrogen base and the linear poly-hydrogen siloxane of chain two ends all containing at least 1 Si-H structure.
Preferably, in described linear poly-hydrogen siloxane, the mass ratio of the first linear poly-hydrogen siloxane and the second linear poly-hydrogen siloxane is 5 ~ 15:2 ~ 20.
Preferably, several side bases of the described first linear poly-hydrogen siloxane are independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl, and have at least 3 side bases to be hydrogen base;
First end group of the described first linear poly-hydrogen siloxane is such as formula shown in (I):
In formula (I), R 1, R 2and R 3independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Second end group of the described first linear poly-hydrogen siloxane is such as formula shown in (II);
In formula (II), R 4, R 5and R 6independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Several side bases of described second linear poly-hydrogen siloxane are independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
First end group of the described second linear poly-hydrogen siloxane is such as formula shown in (III):
In formula (III), R 7and R 8independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Second end group of the described second linear poly-hydrogen siloxane is such as formula shown in (IV):
In formula (IV), R 9and R 10independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl.
Preferably, the viscosity of described linear poly-hydrogen siloxane is 20 ~ 800mPa.s.
Preferably, several side bases of described polysiloxane are independently selected from C 1~ C 18saturated hydrocarbyl, C 1~ C 18replacement saturated hydrocarbyl, C 2~ C 10unsaturated alkyl or C 2~ C 10replacement unsaturated alkyl.
Preferably, described material also comprises hydrophobic modifier.
Preferably, described catalyzer is platinum catalyst; Described inhibitor is alkynyl inhibitor.
The invention provides a kind of preparation method of liquid silastic, comprise the following steps:
A), the inhibitor mixed of the linear poly-hydrogen siloxane of the polysiloxane of 100 ~ 300 weight parts, 0.2 ~ 20 weight part, the white carbon black of 30 ~ 150 weight parts, the catalyzer of 0.002 ~ 0.1 weight part and 0.01 ~ 1 weight part, be heating and curing, obtain liquid silastic;
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
Preferably, described step a) specifically comprises the following steps:
A1), the white carbon black of the polysiloxane of 100 ~ 300 weight parts and 30 ~ 150 weight parts successively through mixing, heating, cooling, obtain liquid silastic base-material;
A2), the catalyst mix of the described liquid silastic base-material of part and 0.002 ~ 0.1 weight part, obtain component A; The linear poly-hydrogen siloxane of liquid silastic base-material described in surplus and 0.2 ~ 20 weight part and the inhibitor mixed of 0.01 ~ 1 weight part, obtain B component;
A3), described component A and B component mixing, be heating and curing, obtain liquid silastic.
Compared with prior art, the invention provides a kind of liquid silastic and preparation method thereof.Liquid silastic provided by the invention is by material successively through mixing, being heating and curing and making, and with weight parts, described material comprises: polysiloxane 100 ~ 300 parts; Linear poly-hydrogen siloxane 0.2 ~ 20 part; White carbon black 30 ~ 150 parts; Catalyzer 0.002 ~ 0.1 part; 0.01 ~ 1 part, inhibitor; Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series; Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane; Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.Liquid silastic provided by the invention with the addition of the linear poly-hydrogen siloxane with special construction in its preparation process, thus makes the liquid silastic obtained have higher tensile strength and tear strength.Experimental result shows, the tensile strength of liquid silastic provided by the invention is not less than 7.0MPa, and tear strength is not less than 18KN/m, B.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of liquid silastic, by material successively through mixing, being heating and curing and making, with weight parts, described material comprises:
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
Liquid silastic provided by the invention is mixed through mixing, heating successively by material, and described material comprises polysiloxane, linear poly-hydrogen siloxane, white carbon black, catalyzer and inhibitor.
In the present invention, described polysiloxane is not containing Si-H structure and has at least 2 substituting groups to be the polysiloxane of unsaturated group of aliphatic series, and namely described polysiloxane is the non-poly-hydrogen siloxane of many unsaturated groups.In an embodiment provided by the invention, several side bases of described polysiloxane are independently selected from C 1~ C 18saturated hydrocarbyl, C 1~ C 18replacement saturated hydrocarbyl, C 2~ C 10unsaturated alkyl or C 2~ C 10replacement unsaturated alkyl.Described C 1~ C 18saturated hydrocarbyl be preferably methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl or decyl; Described C 2~ C 10unsaturated alkyl be preferably C 2~ C 10alkylene, be more preferably vinyl, propenyl, 1-propenyl, butadienyl, hexadienyl, ethenylphenyl or styryl.
In an embodiment provided by the invention, described polysiloxane is cyclic polysiloxanes; In another embodiment provided in the present invention, described polysiloxane is linear polysiloxane, and the first end group of described linear polysiloxane is such as formula shown in (V):
In formula (V), R 11, R 12and R 13independently selected from C 1~ C 18saturated hydrocarbyl, C 1~ C 18replacement saturated hydrocarbyl, C 2~ C 10unsaturated alkyl or C 2~ C 10replacement unsaturated alkyl.Wherein, described C 1~ C 18saturated hydrocarbyl be preferably methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl or decyl; Described C 2~ C 10unsaturated alkyl be preferably C 2~ C 10alkylene, be more preferably vinyl, propenyl, 1-propenyl, butadienyl, hexadienyl, ethenylphenyl or styryl.
Second end group of described linear polysiloxane is such as formula shown in (VI):
In formula (VI), R 14, R 15and R 16independently selected from C 1~ C 18saturated hydrocarbyl, C 1~ C 18replacement saturated hydrocarbyl, C 2~ C 10unsaturated alkyl or C 2~ C 10replacement unsaturated alkyl.Wherein, described C 1~ C 18saturated hydrocarbyl be preferably methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl or decyl; Described C 2~ C 10unsaturated alkyl be preferably C 2~ C 10alkylene, be more preferably vinyl, propenyl, 1-propenyl, butadienyl, hexadienyl, ethenylphenyl or styryl.
In an embodiment provided by the invention, the viscosity of described polysiloxane is 1000 ~ 100000mPa.s; In another embodiment provided by the invention, the viscosity of described polysiloxane is 20000 ~ 90000mPa.s; In other embodiments provided by the invention, the viscosity of described polysiloxane is 20000 ~ 50000mPa.s.
In an embodiment provided by the invention, described polysiloxane is α, ε-vinyl-dimethyl base polydimethylsiloxane and/or multi-vinyl silicone oil.Wherein, described α, ε-vinyl-dimethyl base polydimethylsiloxane is the polydimethylsiloxane that end of the chain Si is connected with 2 methyl with 1 vinyl, and structure is such as formula shown in (VII):
In formula (VII), n represents the polymerization degree.In an embodiment provided by the invention, the viscosity of described α, ε-vinyl-dimethyl base polydimethylsiloxane is 1000 ~ 100000mPa.s; In another embodiment provided by the invention, the viscosity of described α, ε-vinyl-dimethyl base polydimethylsiloxane is 50000 ~ 60000mPa.s.
Described multi-vinyl silicone oil is that vinyl is no less than 3 and end group is the polymethyl siloxane of methyl or vinyl, and structure is such as formula shown in (VIII):
In formula (VIII), a and b represents the polymerization degree, a>=0, b>=0, and a+b ≠ 0; R 17, R 18, R 19, R 20, R 21and R 22independently selected from methyl or vinyl, and formula (VIII) comprises at least 3 vinyl.In an embodiment provided by the invention, the viscosity of described multi-vinyl silicone oil is 20000 ~ 90000mPa.s; In another embodiment provided by the invention, the viscosity of described multi-vinyl silicone oil is 20000 ~ 50000mPa.s.In an embodiment provided by the invention, the molar content of described multi-vinyl silicone oil medium vinyl is 2 ~ 7%.
In an embodiment provided by the invention, described polysiloxane is α, ε-vinyl-dimethyl base polydimethylsiloxane and multi-vinyl silicone oil.The mass ratio of α, ε in described polysiloxane-vinyl-dimethyl base polydimethylsiloxane and multi-vinyl silicone oil is preferably 250 ~ 299:50 ~ 1, is more preferably 285 ~ 294:15 ~ 6.
In an embodiment provided by the invention, the content of polysiloxane described in material is 100 ~ 300 weight parts; In another embodiment provided by the invention, the content of polysiloxane described in material is 250 ~ 300 weight parts.
In the present invention, described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane, and the described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
In an embodiment provided by the invention, several side bases of the described first linear poly-hydrogen siloxane are independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl, and have at least 3 side bases to be hydrogen base;
In an embodiment provided by the invention, the first end group of the described first linear poly-hydrogen siloxane is such as formula shown in (I):
In formula (I), R 1, R 2and R 3independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
In an embodiment provided by the invention, the second end group of the described first linear poly-hydrogen siloxane is such as formula shown in (II);
In formula (II), R 4, R 5and R 6independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
In described first linear poly-hydrogen siloxane, described C 1~ C 18saturated hydrocarbyl be preferably methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl or decyl.
In an embodiment provided by the invention, in the described first linear poly-hydrogen siloxane, the molar content of hydrogen is 0.2 ~ 0.5%; In another embodiment provided by the invention, in the described first linear poly-hydrogen siloxane, the molar content of hydrogen is 0.3 ~ 0.5%.In an embodiment provided by the invention, the viscosity of the described first linear poly-hydrogen siloxane is 20 ~ 800mPa.s; In another embodiment provided by the invention, the viscosity of the described first linear poly-hydrogen siloxane is 50 ~ 130mPa.s.
In an embodiment provided by the invention, the described first linear poly-hydrogen siloxane is trimethylsiloxy group end-blocking polymethyl hydrogen siloxane, and structure is such as formula shown in (IX):
In formula (IX), c and d represents the polymerization degree, c >=0, d > 0.In an embodiment provided by the invention, in described trimethylsiloxy group end-blocking polymethyl hydrogen siloxane, the molar content of hydrogen is 0.2 ~ 0.5%; In another embodiment provided by the invention, in described trimethylsiloxy group end-blocking polymethyl hydrogen siloxane, the molar content of hydrogen is 0.3 ~ 0.5%.In an embodiment provided by the invention, the viscosity of described trimethylsiloxy group end-blocking polymethyl hydrogen siloxane is 20 ~ 800mPa.s; In another embodiment provided by the invention, the viscosity of described trimethylsiloxy group end-blocking polymethyl hydrogen siloxane is 50 ~ 130mPa.s.
In the embodiment that this bright invention provides, described linear poly-hydrogen siloxane also comprises the second linear poly-hydrogen siloxane, and the described second linear poly-hydrogen siloxane is that side base is not hydrogen base and the linear poly-hydrogen siloxane of chain two ends all containing at least 1 Si-H structure.
In an embodiment provided by the invention, several side bases of the described second linear poly-hydrogen siloxane are independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
In an embodiment provided by the invention, the first end group of the described second linear poly-hydrogen siloxane is such as formula shown in (III):
In formula (III), R 7and R 8independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
In an embodiment provided by the invention, the second end group of the described second linear poly-hydrogen siloxane is such as formula shown in (IV):
In formula (IV), R 9and R 10independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl.
In described second linear poly-hydrogen siloxane, described C 1~ C 18saturated hydrocarbyl be preferably methyl, ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, isopentyl, neo-pentyl, tert-pentyl, hexyl, heptyl, octyl group, nonyl or decyl.
In an embodiment provided by the invention, in the described second linear poly-hydrogen siloxane, the molar content of hydrogen is 0.2 ~ 0.5%; In another embodiment provided by the invention, in the described second linear poly-hydrogen siloxane, the molar content of hydrogen is 0.3 ~ 0.5%.In an embodiment provided by the invention, the viscosity of the described second linear poly-hydrogen siloxane is 20 ~ 800mPa.s; In another embodiment provided by the invention, the viscosity of the described second linear poly-hydrogen siloxane is 50 ~ 130mPa.s.
In an embodiment provided by the invention, the described second linear poly-hydrogen siloxane is the polydimethylsiloxane of hydrogen end-blocking, and structure is such as formula shown in (X):
In formula (X), m represents the polymerization degree, R 23, R 24, R 25and R 26independently selected from H or methyl.In an embodiment provided by the invention, in the polydimethylsiloxane of described hydrogen end-blocking, the molar content of hydrogen is 0.2 ~ 0.5%; In another embodiment provided by the invention, in the polydimethylsiloxane of described hydrogen end-blocking, the molar content of hydrogen is 0.3 ~ 0.5%.In an embodiment provided by the invention, the viscosity of the polydimethylsiloxane of described hydrogen end-blocking is 20 ~ 800mPa.s; In another embodiment provided by the invention, the viscosity of the polydimethylsiloxane of described hydrogen end-blocking is 50 ~ 130mPa.s.
In an embodiment provided by the invention, described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane and the second linear poly-hydrogen siloxane, and the mass ratio of the described first linear poly-hydrogen siloxane and the second linear poly-hydrogen siloxane is 5 ~ 15:2 ~ 20; In another embodiment provided by the invention, the mass ratio of the described first linear poly-hydrogen siloxane and the second linear poly-hydrogen siloxane is 5.4 ~ 10.2:2.2 ~ 18.8.
In an embodiment provided by the invention, described in material, the content of linear poly-hydrogen siloxane is 0.2 ~ 20 weight part; In another embodiment provided by the invention, described in material, the content of linear poly-hydrogen siloxane is 5 ~ 24.2 weight parts.
In the present invention, described white carbon black is a kind of reinforced filling in liquid silastic.In an embodiment provided by the invention, the specific surface area of described white carbon black is 200 ~ 400m 2/ g; In another embodiment provided by the invention, the specific surface area of described white carbon black is 200m 2/ g, 250m 2/ g, 300m 2/ g or 400m 2/ g.
In an embodiment provided by the invention, the content of white carbon black described in material is 30 ~ 150 weight parts; In an embodiment provided by the invention, the content of white carbon black described in material is 100 ~ 125 weight parts.
In an embodiment provided by the invention, described material also comprises hydrophobic modifier.In the present invention, the object of adding hydrophobic modifier in material improves the dispersiveness of white carbon black in material.In an embodiment provided by the invention, described hydrophobic modifier comprises hexamethyldisilazane; In another embodiment provided by the invention, described hydrophobic modifier also comprises tetramethyl divinyl disilazane.In an embodiment provided by the invention, the content of described hydrophobic modifier in material is 20 ~ 33wt% of white carbon black content in material; In another embodiment provided by the invention, the content of described hydrophobic modifier in material is 24.8 ~ 28wt% of white carbon black content in material.Comprise in the embodiment of hexamethyldisilazane in a hydrophobic modifier provided by the invention, the content of described hexamethyldisilazane in material is 20 ~ 30wt% of white carbon black content in material; Comprise in the embodiment of hexamethyldisilazane in another hydrophobic modifier provided by the invention, the content of described hexamethyldisilazane in material is 24.8 ~ 25wt% of white carbon black content in material.Comprise in the embodiment of tetramethyl divinyl disilazane in a hydrophobic modifier provided by the invention, the content of described tetramethyl divinyl disilazane in material is 0.1 ~ 3wt% of white carbon black content in material; Comprise in the embodiment of tetramethyl divinyl disilazane in another hydrophobic modifier provided by the invention, the content of described tetramethyl divinyl disilazane in material is 1 ~ 3wt% of white carbon black content in material.
Comprise in the embodiment of hydrophobic modifier at a material provided by the invention, described material also comprises water.In the present invention, the object of adding water in material utilizes water hydrophobic modifier to be decomposed.In an embodiment provided by the invention, the content of described water in material is 20 ~ 25wt% of hydrophobically modified agent content in material.
In an embodiment provided by the invention, described catalyzer is platinum catalyst; In another embodiment provided by the invention, described catalyzer is platinum complex.Be in the embodiment of platinum complex at a catalyzer provided by the invention, the part of described platinum complex is alkene or substituted olefine; Be in the embodiment of platinum complex at another catalyzer provided by the invention, the part of described platinum complex is C 2~ C 8alkene or C 2~ C 8substituted olefine; Be in the embodiment of platinum complex at other catalyzer provided by the invention, the part of described platinum complex is vinylsiloxane; Be in the embodiment of platinum complex at other catalyzer provided by the invention, the part of described platinum complex is 1,3-divinyl-1,1,3,3-tetramethyl disiloxane or 1,3,5,7-tetravinyl-1,3,5,7-tetramethyl-ring siloxanes.
In an embodiment provided by the invention, the content of catalyzer described in material is 0.002 ~ 0.1 weight part; In another embodiment provided by the invention, the content of catalyzer described in material is 0.01 ~ 0.02 weight part.
In an embodiment provided by the invention, described inhibitor is alkynyl inhibitor; In another embodiment provided by the invention, described inhibitor is 1-ethynyl-1-hexalin and/or 2-methyl-3-butyne-2-alcohol and 3,5-dimethyl-1-hexin-3-alcohol.
In an embodiment provided by the invention, the content of inhibitor described in material is 0.01 ~ 1 weight part; In another embodiment provided by the invention, the content of inhibitor described in material is 0.02 ~ 0.04 weight part.
Liquid silastic provided by the invention with the addition of the linear poly-hydrogen siloxane with special construction in its preparation process, thus makes the liquid silastic obtained have higher tensile strength and tear strength.
In preferred implementation provided by the invention, in the process of preparation liquid silastic provided by the invention, with the addition of hydrophobic modifier, preferably with the addition of hexamethyldisilazane and tetramethyl divinyl disilazane.By adding hydrophobic modifier, the surface of the white carbon black in material is made to become hydrophobicity by wetting ability, improve the dispersiveness of white carbon black in material, and make white carbon black to participate in crosslinking reaction, larger strengthening action is served to the network structure of liquid silastic, further increases silicon rubber tear strength.
In preferred implementation provided by the invention, in the process of preparation liquid silastic provided by the invention, with the addition of multi-vinyl silicone oil, the tear strength of liquid silastic goods is strengthened further.
Liquid silicon rubber material applied range provided by the invention, long storage time is not perishable, has higher work-ing life, and prepares the raw material sources that this liquid silastic adopts and be easy to get, and has good industrial prospect.
Experimental result shows, the tensile strength of liquid silastic provided by the invention is not less than 7.0MPa, and tear strength is not less than 18KN/m, B, and hardness (Shao A) is 25 ~ 60, and elongation is 500 ~ 700%.
The invention provides a kind of preparation method of liquid silastic, comprise the following steps:
A), the inhibitor mixed of the linear poly-hydrogen siloxane of the polysiloxane of 100 ~ 300 weight parts, 0.2 ~ 20 weight part, the white carbon black of 30 ~ 150 weight parts, the catalyzer of 0.002 ~ 0.1 weight part and 0.01 ~ 1 weight part, be heating and curing, obtain liquid silastic;
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
In the present invention, directly by polysiloxane, linear poly-hydrogen siloxane, white carbon black, catalyzer and inhibitor mixed, be heating and curing, liquid silastic provided by the invention can be obtained.The consumption of described polysiloxane is 100 ~ 300 weight parts, is preferably 250 ~ 300 weight parts; The consumption of described linear poly-hydrogen siloxane is 0.2 ~ 20 weight part, is preferably 5 ~ 24.2 weight parts; The consumption of described white carbon black is 30 ~ 150 weight parts, is preferably 100 ~ 125 weight parts; The consumption of described catalyzer is 0.002 ~ 0.1 weight part, is preferably 0.01 ~ 0.02 weight part; The consumption of described inhibitor is 0.01 ~ 1 weight part, is preferably 0.02 ~ 0.04 weight part.The described temperature be heating and curing is preferably 120 ~ 150 DEG C; The time of described solidification is preferably 5 ~ 10min.
In an embodiment provided by the invention, prepare in the process of described liquid silastic and also need to add hydrophobic modifier, the consumption of described hydrophobic modifier is preferably 20 ~ 33wt% of white carbon black consumption, is more preferably 24.8 ~ 28wt% of white carbon black consumption.
Add in the embodiment of hydrophobic modifier at one provided by the invention, prepare in the process of described liquid silastic and also need to add water, the consumption of described water is preferably 20 ~ 25wt% of hydrophobic modifier consumption.
In an embodiment provided by the invention, the preparation of described liquid silastic specifically comprises the following steps:
A1), the white carbon black of the polysiloxane of 100 ~ 300 weight parts and 30 ~ 150 weight parts successively through mixing, heating, cooling, obtain liquid silastic base-material;
A2), the catalyst mix of the described liquid silastic base-material of part and 0.002 ~ 0.1 weight part, obtain component A; The linear poly-hydrogen siloxane of liquid silastic base-material described in surplus and 0.2 ~ 20 weight part and the inhibitor mixed of 0.01 ~ 1 weight part, obtain B component;
A3), described component A and B component mixing, be heating and curing, obtain liquid silastic.
In this embodiment, first by polysiloxane and white carbon black mixing.The consumption of described polysiloxane is 100 ~ 300 weight parts, is preferably 250 ~ 300 weight parts; The consumption of described white carbon black is 30 ~ 150 weight parts, is preferably 100 ~ 125 weight parts.The mode of described polysiloxane and white carbon black mixing is preferably mediates; The time of described polysiloxane and white carbon black mixing is preferably 2 ~ 3h; The temperature of described polysiloxane and white carbon black mixing is preferably normal temperature.After described polysiloxane and white carbon black mix, obtain compound.
In the present invention, preferably polysiloxane and white carbon black mixing process in carry out hydrophobic modified to white carbon black, this process specifically comprises:
Polysiloxane, white carbon black, hydrophobic modifier and water are mixed.The consumption of described polysiloxane is 100 ~ 300 weight parts, is preferably 250 ~ 300 weight parts; The consumption of described white carbon black is 30 ~ 150 weight parts, is preferably 100 ~ 125 weight parts; The consumption of described hydrophobic modifier is preferably 20 ~ 33wt% of white carbon black consumption, is more preferably 24.8 ~ 28wt% of white carbon black consumption; The consumption of described water is preferably 20 ~ 25wt% of hydrophobic modifier consumption.The mode of described polysiloxane, white carbon black, hydrophobic modifier and water mixing is preferably mediates; The time of described polysiloxane, white carbon black, hydrophobic modifier and water mixing is preferably 2 ~ 3h; The temperature of described polysiloxane, white carbon black, hydrophobic modifier and water mixing is preferably normal temperature.After described polysiloxane, white carbon black, hydrophobic modifier and water mix, obtain compound.
After obtaining compound, described compound carries out heating successively, cool after, obtain liquid silastic base-material.The temperature of described heating is preferably 150 ~ 160 DEG C.Described heating is preferably carried out under vacuumized conditions, described in the vacuum tightness that vacuumizes preferably be less than or equal to 0.01MPa.In the present invention, preferably pulverize cooling the liquid silastic base-material obtained, the equipment of described pulverizing is preferably three-roller.
After obtained liquid silastic base-material, liquid silastic base-material is divided into two parts, and a copy of it liquid silastic base-material and catalyst mix, obtain component A; Another part of liquid silastic base-material and linear poly-hydrogen siloxane and inhibitor mixed, obtain B component.In the present invention, for ease of distinguishing two parts of liquid silastic base materials, the liquid silastic base material for the preparation of component A is defined as first liquid silicon rubber base material, the liquid silastic base material for the preparation of B component is defined as second liquid silicon rubber base material.The mass ratio of described first liquid silicon rubber base material and second liquid silicon rubber base material is preferably 4 ~ 6:6 ~ 4, is more preferably 1:1.The consumption of described catalyzer is 0.002 ~ 0.1 weight part, is preferably 0.01 ~ 0.02 weight part; The consumption of described linear poly-hydrogen siloxane is 0.2 ~ 20 weight part, is preferably 5 ~ 24.2 weight parts; The consumption of described inhibitor is 0.01 ~ 1 weight part, is preferably 0.02 ~ 0.04 weight part.
In the present invention, for improving obtained component A and the purity of B component, preferably in the process of first liquid silicon rubber base material and catalyst mix and in the process of second liquid silicon rubber base material and linear poly-hydrogen siloxane and inhibitor mixed to mixed system de-bubbled, and to filter after mixing.
After obtaining component A and B component, component A and B component are mixed, is then heating and curing, obtain liquid silastic.The described temperature be heating and curing is preferably 120 ~ 150 DEG C; The time of described solidification is preferably 5 ~ 10min.
Preparation method provided by the invention with the addition of the linear poly-hydrogen siloxane with special construction in liquid silastic preparation process, thus makes the liquid silastic obtained have higher tensile strength and tear strength.
In preferred implementation provided by the invention, in the process preparing liquid silastic, with the addition of hydrophobic modifier.By adding hydrophobic modifier, white carbon black surface is made to become hydrophobicity by wetting ability, improve the dispersiveness of white carbon black in material, and make white carbon black to participate in crosslinking reaction, larger strengthening action is served to the network structure of liquid silastic, further increases silicon rubber tear strength.
Experimental result shows, the tensile strength of liquid silastic provided by the invention is not less than 7.0MPa, and tear strength is not less than 18KN/m, B, and hardness (Shao A) is 25 ~ 60, and elongation is 500 ~ 700%.
For the purpose of clearer, be described in detail below by following examples.
Embodiment 1
300 weight part α are added in vacuum kneader, ε-vinyl-dimethyl base polydimethylsiloxane (viscosity is 50000mPas, 25 DEG C), adds hexamethyldisilazane 25 weight part, water 5 weight part, (specific surface area is 250m to add 100 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 5.0 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 2
300 weight part α are added in vacuum kneader, ε-vinyl-dimethyl base polydimethylsiloxane (viscosity is 50000mPas, 25 DEG C), adds hexamethyldisilazane 28 weight part, water 5.6 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 5.1 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 3
300 weight part α are added in vacuum kneader, ε-vinyl-dimethyl base polydimethylsiloxane (viscosity is 50000mPas, 25 DEG C), adds hexamethyldisilazane 31 weight part, water 6.2 weight part, (specific surface area is 250m to add 125 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.02 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 5.3 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 4
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 1.12 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 7.2 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 5
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 1.68 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 8.3 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 6
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 9.4 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 7
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.8 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 10.5 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 8
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 3.36 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 11.6 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 9
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 9.4 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 4.7 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 10
300 weight part α are added in vacuum kneader, (viscosity is 20000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 9.4 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 4.7 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 11
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 9.4 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 120 DEG C, obtain liquid silicon rubber material.
Embodiment 12
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 9.4 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 130 DEG C, obtain liquid silicon rubber material.
Embodiment 13
294 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), 6 weight part multi-vinyl silicone oil (vinyl molar content 2%, be 20000mPas under viscosity room temperature), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 10.3 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 14
290 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), 10 weight part multi-vinyl silicone oil (vinyl molar content 2%, be 20000mPas under viscosity room temperature), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 10.8 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 15
285 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), 15 weight part multi-vinyl silicone oil (vinyl molar content 2%, be 20000mPas under viscosity room temperature), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 11.6 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 16
276 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), 24 weight part multi-vinyl silicone oil (vinyl molar content 2%, be 20000mPas under viscosity room temperature), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) 13 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 17
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 8 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 9.4 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 18
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 6.7 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 14.1 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 19
300 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 5.4 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 18.8 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 20
285 weight part α are added in vacuum kneader, (viscosity is 50000mPas to ε-vinyl-dimethyl base polydimethylsiloxane, 25 DEG C), 15 weight part multi-vinyl silicone oil (vinyl molar content 2%, be 20000mPas under viscosity room temperature), add hexamethyldisilazane 28 weight part, water 5.6 weight part, add tetramethyl divinyl disilazane 2.24 weight part, (specific surface area is 250m to add 112 weight part white carbon blacks 2/ g), mix, normal temperature mediates 2h, is then warming up to 150 DEG C, vacuumizes de-low molecule 3h, after cooling, through three-roller grinding, filters, finally obtains liquid silastic base-material.
Aforesaid liquid silicon rubber base-material is divided into two parts, and in a liquid silastic base-material, add 1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.01 weight part, stir de-bubbled, filters, obtained component (A); Trimethylsiloxy group end-blocking polymethyl hydrogen siloxane (viscosity 130mPas is added in another part of liquid silastic base-material, 25 DEG C, H mol%=0.3mol%) polydimethylsiloxane (the viscosity 50mPas of 10.2 weight parts and hydrogen end-blocking, 25 DEG C, H mol%=0.2mol%) 2.2 weight parts and 1-ethynyl-1-hexalin reaction suppressor 0.04 weight part, at room temperature mix, de-bubbled, filter, obtained component (B).
Above-mentioned obtained component (A) and component (B) are mixed, is expelled in mould, heat 5min solidification at 150 DEG C, obtain liquid silicon rubber material.
Embodiment 21
Performance test
Liquid silicon rubber material obtained for embodiment 1 ~ 20 is made the thick film of 6mm be used for carrying out hardness test (standard GB/T531.1-2008); Make the thick film of 2mm to be used for carrying out physical and mechanical property test (tensile strength and elongation measure by GB/T528-1998, and tear strength is pressed GB/T529-1999 and measured), experimental result is in table 1,2 and 3.
Table 1 physical and mechanical properties test-results
Embodiment Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7
Hardness (Shao A) 30 38 45 42 43 46 47
Tensile strength (MPa) 7.5 8.5 8.8 8.3 8.0 8.2 8.0
Elongation (%) 650 660 630 640 600 590 580
Tear strength (KN/m, B) 20 25 28 33 36 40 43
Table 2 physical and mechanical properties test-results
Embodiment Embodiment 8 Embodiment 9 Embodiment 10 Embodiment 11 Embodiment 12 Embodiment 13 Embodiment 14
Hardness (Shao A) 47 43 41 43 45 50 52
Tensile strength (MPa) 7.5 8.8 8.5 8.4 8.1 7.8 7.5
Elongation (%) 500 620 590 620 610 570 550
Tear strength (KN/m, B) 39 42 39 38 38 44 46
Table 3 physical and mechanical properties test-results
Embodiment Embodiment 15 Embodiment 16 Embodiment 17 Embodiment 18 Embodiment 19 Embodiment 20
Hardness (Shao A) 55 60 43 38 29 54
Tensile strength (MPa) 7.3 7.0 8.4 8.6 8.8 8.9
Elongation (%) 530 500 620 630 660 550
Tear strength (KN/m, B) 49 47 38 35 18 50
Can be found out by upper table, liquid silastic provided by the invention has higher tensile strength and tear strength.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (10)

1. a liquid silastic, by material successively through mixing, being heating and curing and making, with weight parts, described material comprises:
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
2. liquid silastic according to claim 1, is characterized in that, described linear poly-hydrogen siloxane also comprises the second linear poly-hydrogen siloxane;
Described second linear poly-hydrogen siloxane is that side base is not hydrogen base and the linear poly-hydrogen siloxane of chain two ends all containing at least 1 Si-H structure.
3. liquid silastic according to claim 2, is characterized in that, in described linear poly-hydrogen siloxane, the mass ratio of the first linear poly-hydrogen siloxane and the second linear poly-hydrogen siloxane is 5 ~ 15:2 ~ 20.
4. liquid silastic according to claim 2, is characterized in that, several side bases of the described first linear poly-hydrogen siloxane are independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl, and have at least 3 side bases to be hydrogen base;
First end group of the described first linear poly-hydrogen siloxane is such as formula shown in (I):
In formula (I), R 1, R 2and R 3independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Second end group of the described first linear poly-hydrogen siloxane is such as formula shown in (II);
In formula (II), R 4, R 5and R 6independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Several side bases of described second linear poly-hydrogen siloxane are independently selected from C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
First end group of the described second linear poly-hydrogen siloxane is such as formula shown in (III):
In formula (III), R 7and R 8independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl;
Second end group of the described second linear poly-hydrogen siloxane is such as formula shown in (IV):
In formula (IV), R 9and R 10independently selected from hydrogen base, C 1~ C 18saturated hydrocarbyl or C 1~ C 18replacement saturated hydrocarbyl.
5. liquid silastic according to claim 1, is characterized in that, the viscosity of described linear poly-hydrogen siloxane is 20 ~ 800mPa.s.
6. liquid silastic according to claim 1, is characterized in that, several side bases of described polysiloxane are independently selected from C 1~ C 18saturated hydrocarbyl, C 1~ C 18replacement saturated hydrocarbyl, C 2~ C 10unsaturated alkyl or C 2~ C 10replacement unsaturated alkyl.
7. liquid silastic according to claim 1, is characterized in that, described material also comprises hydrophobic modifier.
8. liquid silastic according to claim 1, is characterized in that, described catalyzer is platinum catalyst; Described inhibitor is alkynyl inhibitor.
9. a preparation method for liquid silastic, comprises the following steps:
A), the inhibitor mixed of the linear poly-hydrogen siloxane of the polysiloxane of 100 ~ 300 weight parts, 0.2 ~ 20 weight part, the white carbon black of 30 ~ 150 weight parts, the catalyzer of 0.002 ~ 0.1 weight part and 0.01 ~ 1 weight part, be heating and curing, obtain liquid silastic;
Described polysiloxane does not contain Si-H structure and has at least 2 substituting groups to be unsaturated group of aliphatic series;
Described linear poly-hydrogen siloxane comprises the first linear poly-hydrogen siloxane;
Described first linear poly-hydrogen siloxane is that the end of the chain has at least 3 side bases to be the linear poly-hydrogen siloxane of hydrogen base not containing Si-H structure.
10. preparation method according to claim 9, is characterized in that, described step a) specifically comprises the following steps:
A1), the white carbon black of the polysiloxane of 100 ~ 300 weight parts and 30 ~ 150 weight parts successively through mixing, heating, cooling, obtain liquid silastic base-material;
A2), the catalyst mix of the described liquid silastic base-material of part and 0.002 ~ 0.1 weight part, obtain component A; The linear poly-hydrogen siloxane of liquid silastic base-material described in surplus and 0.2 ~ 20 weight part and the inhibitor mixed of 0.01 ~ 1 weight part, obtain B component;
A3), described component A and B component mixing, be heating and curing, obtain liquid silastic.
CN201510217623.9A 2015-04-30 2015-04-30 Liquid silicon rubber and preparation method thereof Pending CN104817845A (en)

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CN110591386A (en) * 2019-09-03 2019-12-20 四川大学 A curable insulating vinyl silicone grease material and its preparation method and application
CN113444369A (en) * 2021-06-28 2021-09-28 浙江新安化工集团股份有限公司 Bi-component liquid silicone rubber and preparation method thereof

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