CN105273410A - Preparation method of high-elasticity addition silicone rubber - Google Patents
Preparation method of high-elasticity addition silicone rubber Download PDFInfo
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- CN105273410A CN105273410A CN201510742672.4A CN201510742672A CN105273410A CN 105273410 A CN105273410 A CN 105273410A CN 201510742672 A CN201510742672 A CN 201510742672A CN 105273410 A CN105273410 A CN 105273410A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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Abstract
The invention discloses a preparation method of high-elasticity addition silicone rubber. The preparation method comprises the following steps: uniformly mixing vinyl polysiloxane, nanosilicon dioxide, polysiloxane, silicon resin, a platinum catalyst, a hydrosilylation reaction inhibitor and hydrogen-containing silicone oil according to a ratio, then curing a mixture prepared after uniformly mixing at 70-200 DEG C to prepare the high-elasticity addition silicone rubber. The high-elasticity addition silicone rubber prepared by the method has excellent heat resistance; the heat resistance temperature of the high-elasticity addition silicone rubber can reach up to 400 DEG C; the high-elasticity addition silicone rubber has excellent mechanical property; the tensile elongation can reach over 1000%; meanwhile, the high-elasticity addition silicone rubber has the resistance to ageing, is long in service life and can be widely used in the fields such as medical treatment, aerospace, electronics and historic preservation. The preparation method is simple, low in cost and free of pollution to ecological environment.
Description
Technical field
The present invention relates to organic polymer material field, particularly relate to a kind of preparation method of snappiness addition silicon rubber.
Background technology
Addition-type silicon rubber is a kind of excellent specialty elastomer, is generally addition-crosslinked and form elastomer material under platinum catalyst effect by the vinyl in rubber and the silicon hydrogen base in linking agent.Compare with hot radical cure silicone rubber with condensed type, this kind of silicon rubber does not discharge small molecules in sulfidation, there is after sulfuration little, nontoxic, the good wet fastness of shrinking percentage, low incendivity, can the high and vulcanization rate of degree of depth sulfuration, physical strength can, by advantages such as temperature control, be the class silicon rubber greatly developed both at home and abroad at present.Addition-type silicon rubber in the curing process, no coupling product generates, shrinking percentage is minimum, the advantages such as energy deep cure, and its mechanical property is between two kinds of silicon rubber, be widely used in the fields such as medical treatment, apparatus, electronic apparatus, chemical industry, wrapping material and aerospace, copying and the fields such as renderings of artistic handicrafts particularly at historical relic, is used to make the excellent material of imitated mould.But along with the development of science and technology, its resistance to thermal degradation performance and mechanical property are had higher requirement.
In order to improve mechanical property and the Heat-resistant stable performance of silicon rubber, various toughener as: clay carbon black, white carbon black, carbon nanotube, polyhedral oligomeric silsesquioxane and Graphene etc. are widely used in and improve the mechanical property of silicon rubber and thermal stability.Chinese Patent Application No. 201410627311.0, publication date is on February 4th, 2015, and name is called " a kind of cable flame-proof silicon rubber ", the silicon rubber that the method adopts the methyl ethylene dimethione of high molecular to prepare, but poor mechanical property, elongation at break just reaches 400%.Chinese Patent Application No. 201210296531.0, publication date is on December 19th, 2012, and name is called " a kind of liquid silastic ", and the method claims that the Mechanical Properties of Silicone Rubber of preparation is relatively good, but elongation at break maintains about 500%.Chinese Patent Application No. 201410856778.2, publication date is on 03 25th, 2015, name is called " add-on type liquid silicon rubber and preparation method thereof ", this patent claims adopts MDQ silicone resin to be the silicon rubber that unique toughener can prepare excellent in mechanical performance, elongation at break reaches as high as 800%, and its effect makes us being difficult to convince really.In a word, commercially the elongation at break of the silicon rubber of various kind maintains between 200% ~ 500% substantially, and heat-resisting unsatisfactory with weathering resistance, the excellent mechanical property that many silicone rubber products obtain is based upon on the basis of its heat resistance of reduction often.
Summary of the invention
For the problems referred to above, the object of the present invention is to provide a kind of preparation method of snappiness addition silicon rubber.
To achieve these goals, technical solution of the present invention is,
A preparation method for snappiness addition silicon rubber, described method is carried out according to the following steps:
By following parts by weight:
Vinyl polysiloxane 50 ~ 100 parts;
Nano silicon 0.5-10 part;
Polysiloxane 5 ~ 100 parts;
Silicone resin 1 ~ 30 part;
Platinum catalyst 0.00015 ~ 0.1 part;
Addition reaction of silicon with hydrogen inhibitor, its content is the coordinating group of 1 ~ 100mol that described platinum catalyst per molecule Pt is corresponding;
Containing hydrogen silicone oil 1.18 ~ 10 parts;
After said components is mixed in vacuum kneader or Banbury mixer, at 70 ~ 200 DEG C, solidify 0.1 ~ 3h obtain.
Described vinyl polysiloxane is a kind of or end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane the proportioning in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane is the complex body of 1:1 ~ 10, wherein, the molecular-weight average of end-vinyl polydimethylsiloxane is 1.0 ~ 640,000, polyvinyl methylsiloxane molecular-weight average is 0.5 ~ 640,000, the contents of ethylene 0.02mol ~ 1.10mol/100g in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane.
Described nano silicon is one or both in conventional hydrophobic or hydrophilic gas-phase silica or precipitated silica or silicon sol, and its particle dia is 5 ~ 1000nm.
Described polysiloxane has following structural formula:
R in formula
1for hydrogen atom or methyl or vinyl, R
2for hydrogen atom or methyl or vinyl or phenyl.
Described silicone resin is the one in liquid MQ silicone resin or MTQ silicone resin or MDQ silicone resin or MT silicone resin, and its viscosity is at 5 ~ 1000cSt.
Described Pt catalyzer is the aqueous isopropanol or 1 of Platinic chloride, 3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex or two (alkynyls) (1,5-cyclooctadiene) platinum complex or two (alkynyls) (two rings [2.2.1] heptan-2,5-diene) platinum complex or two (alkynyls) (1,5-dimethyl-1,5-cyclooctadiene) platinum complex or two (alkynyls) (1,6-dimethyl-1,5-cyclooctadiene) one in platinum complex or diethyl phthalate platinum complex.
Described addition reaction of silicon with hydrogen inhibitor is the one in 3-methyl isophthalic acid-butine-3-alcohol or 1-ethynylcyclohexanol or 3-phenyl-1-butyl-3-alcohol or 3,5-dimethyl-1-hexin-3-alcohol or 3-octyl group-ethyl acetylene-3-alcohol or t etram-ethyltetravinylcyclotetrasiloxane.
In described containing hydrogen silicone oil, hydrogen richness is 0.5 ~ 1.55%, and during room temperature, viscosity is at 10 ~ 50cSt.
Owing to have employed above technical scheme, the preparation method of a kind of snappiness addition silicon rubber of the present invention, its beneficial effect is:
(1) addition-type silicon rubber that prepared by the present invention evenly spreads in polysiloxane by nano silicon on the basis of existing silicon rubber, because nano silicon has sizable specific surface area, it is made to play the effect of cross-linking set at silicon rubber, thus make the vinyl polysiloxane chain in silicon rubber appropriately crosslinked, but also can by controlling nano silicon and silicone resin consumption adjustment addition silicon rubber elastic.
(2) preparation method of the present invention is simple; the snappiness addition silicon rubber of preparation has good thermotolerance; its heat resisting temperature can reach 400 DEG C; and the mechanical property of excellence; its elongation at break can more than 1000%; and can be anti-aging, long service life, can be widely used in the fields such as medical treatment, aerospace, electronics and historical relic's protection.
Embodiment
With specific embodiment, the invention will be further described below, but the present invention is not by the restriction of following embodiment.
A preparation method for snappiness addition silicon rubber, described method is carried out according to the following steps:
By following parts by weight:
Vinyl polysiloxane 50 ~ 100 parts;
Nano silicon 0.5-10 part;
Polysiloxane 5 ~ 100 parts;
Silicone resin 1 ~ 30 part;
Platinum catalyst 0.00015 ~ 0.1 part;
Addition reaction of silicon with hydrogen inhibitor, its content is the coordinating group of 1 ~ 100mol that described platinum catalyst per molecule Pt is corresponding;
Containing hydrogen silicone oil 1.18 ~ 10 parts;
After said components is mixed in vacuum kneader or Banbury mixer, at 70 ~ 200 DEG C, solidify 0.1 ~ 3h obtain.
Wherein: vinyl polysiloxane is a kind of or end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane the proportioning in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane is the complex body of 1:1 ~ 10, wherein, the molecular-weight average of end-vinyl polydimethylsiloxane is 1.0 ~ 640,000, polyvinyl methylsiloxane molecular-weight average is 0.5 ~ 640,000, the contents of ethylene 0.02mol ~ 1.10mol/100g in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane; Nano silicon is one or both in conventional hydrophobic or hydrophilic gas-phase silica or precipitated silica or silicon sol, and wherein, conventional hydrophobic or hydrophilic gas-phase silica or precipitated silica particle dia are 5 ~ 1000nm.Polysiloxane has following structural formula:
R in formula
1for hydrogen atom, methyl, vinyl etc., R
2for hydrogen atom, methyl, vinyl, phenyl etc.Why select described siloxanes, be because: siloxane polymer is made up of different types of compound, comprises traditional silicone oil, water-soluble polymers, oil-soluble polymers, fluorine soluble polymer and has the polymkeric substance of multiple solubleness.They exist with various different form, from low viscosity fluid to having elastic elastomerics and synthetic resins.And R
1for hydrogen atom, methyl, vinyl etc., R
2polysiloxane for hydrogen atom, methyl, vinyl, phenyl has good snappiness.Silicone resin is the one in liquid MQ silicone resin or MTQ silicone resin or MDQ silicone resin or MT silicone resin, and its viscosity is at 5 ~ 1000cSt.Pt catalyzer is the aqueous isopropanol or 1 of Platinic chloride, 3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex or two (alkynyls) (1,5-cyclooctadiene) platinum complex or two (alkynyls) (two rings [2.2.1] heptan-2,5-diene) platinum complex or two (alkynyls) (1,5-dimethyl-1,5-cyclooctadiene) platinum complex or two (alkynyls) (1,6-dimethyl-1,5-cyclooctadiene) one in platinum complex or diethyl phthalate platinum complex.Addition reaction of silicon with hydrogen inhibitor is the one in 3-methyl isophthalic acid-butine-3-alcohol or 1-ethynylcyclohexanol or 3-phenyl-1-butyl-3-alcohol or 3,5-dimethyl-1-hexin-3-alcohol or 3-octyl group-ethyl acetylene-3-alcohol or t etram-ethyltetravinylcyclotetrasiloxane.In containing hydrogen silicone oil, hydrogen richness is 0.5 ~ 1.55%, and during room temperature, viscosity is at 10 ~ 50cSt.The addition-type silicon rubber prepared due to the method successfully evenly spreads in polysiloxane by nano silicon on the basis of existing silicon rubber, utilize the specific surface area that nano material is high, make nano silicon play the effect of cross-linking set at silicon rubber, thus make the vinyl polysiloxane chain in silicon rubber appropriately crosslinked.Meanwhile, the elasticity of silicon rubber can also be improved by the regulation and control particle diameter of nano silicon and the consumption of nano silicon and silicon rubber.The snappiness addition silicon rubber adopting the method to prepare has good thermotolerance; its heat resisting temperature can reach 400 DEG C; and the mechanical property of excellence; its elongation at break can more than 1000%; and can be anti-aging; long service life, can be widely used in the fields such as medical treatment, aerospace, electronics and historical relic's protection.
By above-mentioned preparation method:
Embodiment 1
By following parts by weight:
End-vinyl polydimethylsiloxane 50 parts;
Particle diameter is the conventional dewatering nano gas-phase silica 0.5 part of 5nm;
R
1and R
2be the polysiloxane 5 parts of hydrogen atom;
Viscosity is the MQ silicone resin 1 part of 5cSt;
The aqueous isopropanol of Platinic chloride 0.00015 part;
3-methyl isophthalic acid-butine-3-alcohol 0.02 part;
Hydrogen richness is 0.5%, and during room temperature, viscosity is at 1.18 parts of 10cSt containing hydrogen silicone oil;
Said components mixed in vacuum kneader, and solidify 0.1h at 70 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1000%.
Embodiment 2
By following parts by weight:
Polyvinyl methylsiloxane 60 parts;
Particle diameter is the conventional hydrophilic nano-gas-phase white carbon black 2 parts of 30nm;
R
1and R
2be the polysiloxane 20 parts of methyl;
Viscosity is the MTQ silicone resin 5 parts of 70cSt;
1,3-divinyl-1,1,3,3-tetramethyl disiloxane platinum complex 0.0003 part;
Hydrogen richness is 0.72%, and during room temperature, viscosity is at 2 parts of 15cSt containing hydrogen silicone oil;
Said components mixed in vacuum kneader, and solidify 0.25h at 80 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1280%.
Embodiment 3
By following parts by weight:
The proportioning of end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane is the complex body 70 parts of 1:1;
Particle diameter is the precipitated silica 3.5 parts of 100nm;
R
1and R
2be the polysiloxane 20 parts of vinyl;
Viscosity is the MDQ silicone resin 5 parts of 120cSt;
Two (alkynyls) (1,5-cyclooctadiene) platinum complex 0.00072 part;
3-phenyl-1-butyl-3-alcohol 1.02 parts
Hydrogen richness is 0.95%, and during room temperature, viscosity is at 2 parts of 22cSt containing hydrogen silicone oil;
Said components mixed in vacuum kneader, and solidify 0.5h at 95 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1066%.
Embodiment 4
By following parts by weight:
The proportioning of end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane is the complex body 80 parts of 1:3;
Particle diameter is 5 parts, the silicon sol alkane of 175nm;
R
1and R
2be respectively the polysiloxane 60 parts of hydrogen atom and phenyl;
Viscosity is the MT silicone resin 13 parts of 300cSt;
Two (alkynyls) (diene in two rings [2.2.1] heptan-2,5-) platinum complex 0.001 part;
3,5-dimethyl-1-hexin-3-alcohol 1.15 parts;
Hydrogen richness is 1.08%, and during room temperature, viscosity is at the containing hydrogen silicone oil 4 parts of 30cSt;
Said components mixed in vacuum kneader, and solidify 1h at 100 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1325%.
Embodiment 5
By following parts by weight:
The proportioning of end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane is the complex body 88 parts of 1:6;
Silicon sol 6 parts;
R
1and R
2be respectively the polysiloxane 75 parts of methyl and phenyl;
Viscosity is the MT silicone resin 20 parts of 500cSt;
Two (alkynyls) (1,5-dimethyl-1,5-cyclooctadiene) platinum complex 0.008 part;
3-octyl group-ethyl acetylene-3-alcohol 1.24 parts;
Hydrogen richness is 1.15%, and during room temperature, viscosity is at the containing hydrogen silicone oil 5 parts of 35cSt;
Said components mixed in Banbury mixer, and solidify 1.5h at 125 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1430%.
Embodiment 6
By following parts by weight:
The proportioning of end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane is the complex body 95 parts of 1:8;
Silicon sol 8 parts;
R
1and R
2be respectively the polysiloxane 80 parts of vinyl and phenyl;
Viscosity is the MT silicone resin 24 parts of 750cSt;
Two (alkynyls) (1,6-dimethyl-1,5-cyclooctadiene) platinum complex 0.032 part;
T etram-ethyltetravinylcyclotetrasiloxane 1.35 parts;
Hydrogen richness is 1.32%, and during room temperature, viscosity is at the containing hydrogen silicone oil 8 parts of 43cSt;
Said components mixed in Banbury mixer, and solidify 2h at 150 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1168%.
Embodiment 7
By following parts by weight:
The proportioning of end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane is the complex body 100 parts of 1:10;
Silicon sol 10 parts;
R
1and R
2be respectively the polysiloxane 100 parts of methyl and vinyl;
Viscosity is the MT silicone resin 30 parts of 1000cSt;
Diethyl phthalate platinum complex 0.1 part;
T etram-ethyltetravinylcyclotetrasiloxane 1.412 parts;
Hydrogen richness is 1.55%, and during room temperature, viscosity is at the containing hydrogen silicone oil 10 parts of 50cSt;
Said components mixed in Banbury mixer, and solidify 3h at 200 DEG C, obtain snappiness addition silicon rubber, the elongation at break of this snappiness addition silicon rubber can reach 1542%.
Claims (8)
1. a preparation method for snappiness addition silicon rubber, is characterized in that: described method is carried out according to the following steps:
By following parts by weight:
Vinyl polysiloxane 50 ~ 100 parts;
Nano silicon 0.5-10 part;
Polysiloxane 5 ~ 100 parts;
Silicone resin 1 ~ 30 part;
Platinum catalyst 0.00015 ~ 0.1 part;
Addition reaction of silicon with hydrogen inhibitor, its content is the coordinating group of 1 ~ 100mol that described platinum catalyst per molecule Pt is corresponding;
Containing hydrogen silicone oil 1.18 ~ 10 parts;
After said components is mixed in vacuum kneader or Banbury mixer, at 70 ~ 200 DEG C, solidify 0.1 ~ 3h obtain.
2. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, it is characterized in that: described vinyl polysiloxane is a kind of or end-vinyl polydimethylsiloxane and polyvinyl methylsiloxane the proportioning in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane is the complex body of 1:1 ~ 10, wherein, the molecular-weight average of end-vinyl polydimethylsiloxane is 1.0 ~ 640,000, polyvinyl methylsiloxane molecular-weight average is 0.5 ~ 640,000, contents of ethylene 0.02mol ~ 1.10mol/100g in end-vinyl polydimethylsiloxane or polyvinyl methylsiloxane.
3. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, it is characterized in that: described nano silicon is one or both in conventional hydrophobic or hydrophilic gas-phase silica or precipitated silica or silicon sol, and its particle dia is 5 ~ 1000nm.
4. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, is characterized in that: described polysiloxane has following structural formula:
R in formula
1for hydrogen atom or methyl or vinyl, R
2for hydrogen atom or methyl or vinyl or phenyl.
5. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, is characterized in that: described silicone resin is the one in liquid MQ silicone resin or MTQ silicone resin or MDQ silicone resin or MT silicone resin, and its viscosity is at 5 ~ 1000cSt.
6. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, it is characterized in that: described Pt catalyzer is the aqueous isopropanol or 1 of Platinic chloride, 3-divinyl-1, 1, 3, 3-tetramethyl disiloxane platinum complex or two (alkynyls) (1, 5-cyclooctadiene) platinum complex or two (alkynyls) (two rings [2.2.1] heptan-2, 5-diene) platinum complex or two (alkynyls) (1, 5-dimethyl-1, 5-cyclooctadiene) platinum complex or two (alkynyls) (1, 6-dimethyl-1, 5-cyclooctadiene) one in platinum complex or diethyl phthalate platinum complex.
7. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, it is characterized in that: described addition reaction of silicon with hydrogen inhibitor is the one in 3-methyl isophthalic acid-butine-3-alcohol or 1-ethynylcyclohexanol or 3-phenyl-1-butyl-3-alcohol or 3,5-dimethyl-1-hexin-3-alcohol or 3-octyl group-ethyl acetylene-3-alcohol or t etram-ethyltetravinylcyclotetrasiloxane.
8. the preparation method of a kind of snappiness addition silicon rubber according to claim 1, is characterized in that: in described containing hydrogen silicone oil, hydrogen richness is 0.5 ~ 1.55%, and during room temperature, viscosity is at 10 ~ 50cSt.
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| CN110957078A (en) * | 2019-12-17 | 2020-04-03 | 东莞市骏豪电线科技有限公司 | Manufacturing method of multi-color silica gel doubling and electric wire thereof |
| CN113652090A (en) * | 2021-04-27 | 2021-11-16 | 江门市胜鹏化工实业有限公司 | Liquid silicone rubber composition and method for preparing silicone rubber |
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