CN103319900A - High-transparency room-temperature-cured silicone composition and preparation method thereof - Google Patents
High-transparency room-temperature-cured silicone composition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a silicone composition, and especially relates to a high-transparency room-temperature-cured silicone composition and a preparation method thereof. The composition is used as a sealant and adhesive. The composition is prepared from the components of, by mass, 100 parts of hydroxy-terminated polydimethylsiloxane, 0-50 parts of alkyl-terminated polydimethylsiloxane, 3-20 parts of gas-phase silica, 0.000001-0.0001 parts of an organic fluorescent agent, 1-50 parts of polyisobutylene, 1-20 parts of a crosslinking aagent, 0.1-2 parts of a coupling agent, and 0.01-0.2 parts of a catalyst. The composition is obtained through vacuuming and stirring. According to the high-transparency room-temperature-cured silicone composition and the preparation method thereof, the composition has high transparency, improved quality, and improved application grade.
Description
Technical field
The present invention relates to a kind of silicon-ketone composition, relate in particular to a kind of high transparent self-vulcanizing silicon-ketone composition and preparation method thereof, as sealing agent and tackiness agent.
Background technology
Must add reinforced filling in the self-vulcanizing silicon composition of the prior art, mostly be aerosil and nano-calcium carbonate, in fact most of nano-metal-oxides all have strengthening action to it.Formulation without the reinforcement filler can be made into transparence, is the jelly shape after solidifying,, nonelastic without intensity, application is restricted.Reinforced filling is transparent influential to composition, is that the composition of reinforced filling can be made into translucent (or being called oyster white) seal gum with aerosil, and the composition made from other reinforced filling is opaque.
Needing tackiness agent or sealing agent in the actual application is all-transparent, as: the high penetration glass curtain wall, seal with high transparent sealing glue between the glass, visual effect, glass and the crystal works bonding, high-grade jewellery exhibition cabinet bonding, the saturating lamp of all-pass that have a kind of whole glass are decorated bonding, LED encapsulation, LED is excellent because of its energy-saving effect, be used widely at aspects such as illumination, outdoor display screen, advertising lamp, ornament lamp, instrument pilot lamp in recent years, at the encapsulation of LED product, embedding, sealing agent and the binding agent that needs all-transparent such as bonding.The organosilicon sealant transparency of selling in the market is not high, mostly is translucent product.
Summary of the invention
The present invention solves the deficiencies in the prior art, and a kind of raising composition transparency is provided, and strengthens ageing-resistant bosom and stable on heating a kind of high transparent self-vulcanizing silicon-ketone composition and preparation method thereof.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
A kind of high transparent self-vulcanizing silicon-ketone composition, carry out proportioning by following mass parts:
100 parts of hydroxyl endblocked polydimethylsiloxanes;
0～50 part of alkyl-blocked polydimethylsiloxane;
3～20 parts of aerosils;
0.000001～0.0001 part of organic fluorescence agent;
1～50 part of polyisobutene;
1～20 part of linking agent;
0.1～2 part of coupling agent;
0.01～0.2 part of catalyzer.
As preferably, the viscosity of described hydroxyl endblocked polydimethylsiloxane when temperature is 25 ℃ is 0.5～200Pa.S.
As preferably, the specific surface area of described aerosil is 300～500m
2/ g.
As preferably, process with silazane or methyl chlorosilane on the surface of described aerosil.
As preferably, described organic fluorescence agent is colourless organic compound, and the organic fluorescence agent can absorbing wavelength be the ultraviolet ray of 300～400nm, and radiating wavelength is the bluish voilet fluorescence of 420～480nm.
As preferably, described organic fluorescence agent is one or more the mixture in distyryl biphenyl class, coumarins, the Phthalimide class fluorescent agent;
Described coupling agent is one or more the mixture in aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl trimethoxysilane, N-β aminoethyl γ aminopropyl trimethoxysilane, the 3-glycidyl ether oxygen base propyl trimethoxy silicane;
Described catalyzer is one or more the mixture in dibutyl tin laurate, dibutyltin diacetate, Dibutyltin oxide, the ethyl-diacetyl-acetate diisopropoxy titanium.
As preferably, described polyisobutene is low-molecular weight polymer, and the polymerization degree of polyisobutene is 3～300, and the viscosity of polyisobutene is 0.002～2Pa.s.
As preferably, described linking agent is one or more the mixture in methyltrimethoxy silane, vinyltrimethoxy silane, tetramethoxy-silicane, Union carbide A-162, methyl triacetoxysilane, vinyltriacetoxy silane, tetrem acyloxy silane, methyl tributanoximo silane, vinyl three ketoximinosilanes, phenyl tributanoximo silane, four Diacetylmonoxime base silanes, methyl three (methyl isobutyl ketoxime base) silane.
As preferably, when described linking agent was methyl three (methyl isobutyl ketoxime base) silane, the molecular formula of methyl three (methyl isobutyl ketoxime base) silane was: C19H39N3SI03
A kind of preparation method of high transparent self-vulcanizing silicon-ketone composition, carry out according to the following steps:
(1), in the equipment that can vacuumize, disperse with brute force oar, adds hydroxyl endblocked polydimethylsiloxane, polyisobutene, organic fluorescence agent, stir, the speed that stirs is 300～1000 to turn, suction in the equipment is-0.06～-0.1MPa, the time of stirring is 5～30min;
(2), after the step (1), in equipment, add linking agent, stir, the speed of stirring is 300～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 5～30min;
(3), after the step (2), in equipment, add aerosil, stir, stirring velocity is 600～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 10～30min;
(4), after the step (3), in equipment, add coupling agent, stir, the speed of stirring is 600～1000 to turn again, the suction in the equipment-0.06～-0.1MPa, the time of stirring is 10～20min;
(5), after the step (4), in equipment, add catalyzer, stir, the speed of stirring is 600～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 10～20min;
(6), pack after the discharging, place and carry out the transparency test after 72 hours, the testing method of transparency is: seal gum is made 5mm thickness film, be placed on after the curing on the blank sheet of paper of No. 5 words of the Song typeface, see through film and see word on the blank sheet of paper, being placed on the paper effect with the 5mm float glass equally is 1, is placed on the 10mm float glass that effect equally is 2 on the paper, the font of seeing some fuzzy be 3, distinguish that misknowing word content is 4, can only see that fuzzy word shadow is 5, word that can't see the back fully is 6.
The transparency of numeral 1 is best, and the transparency of numeral 6 is the poorest.
Therefore, a kind of high transparent self-vulcanizing silicon-ketone composition of the present invention and preparation method thereof possesses high-clarity, and Improving The Quality of Products improves and uses class.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: a kind of high transparent self-vulcanizing silicon-ketone composition, carry out proportioning by following mass parts:
100 parts of hydroxyl endblocked polydimethylsiloxanes;
0 part of alkyl-blocked polydimethylsiloxane;
3 parts of aerosils;
0.000001 part of organic fluorescence agent;
1 part of polyisobutene;
1 part of linking agent;
0.1 part of coupling agent;
0.01 part of catalyzer.
The viscosity of described hydroxyl endblocked polydimethylsiloxane when temperature is 25 ℃ is 0.5Pa.S.
The specific surface area of described aerosil is 300m
2/ g.
Process with silazane or methyl chlorosilane on the surface of described aerosil.
Described organic fluorescence agent is colourless organic compound, and the organic fluorescence agent can absorbing wavelength be the ultraviolet ray of 300nm, and radiating wavelength is the bluish voilet fluorescence of 420nm.
Described organic fluorescence agent is the distyryl biphenyl class;
Described coupling agent is aminopropyl trimethoxysilane;
Described catalyzer is dibutyl tin laurate.
Described polyisobutene is low-molecular weight polymer, and the polymerization degree of polyisobutene is 3, and the viscosity of polyisobutene is 0.002Pa.s.
Described linking agent is methyltrimethoxy silane.
When described linking agent was methyl three (methyl isobutyl ketoxime base) silane, the molecular formula of methyl three (methyl isobutyl ketoxime base) silane was: C19H39N3SI03
A kind of preparation method of high transparent self-vulcanizing silicon-ketone composition, carry out according to the following steps:
(1), in the equipment that can vacuumize, disperse with brute force oar, adds hydroxyl endblocked polydimethylsiloxane, polyisobutene, organic fluorescence agent, stir, the speed that stirs is 300 to turn, and the suction in the equipment is-0.06MPa that the time of stirring is 5min;
(2), after the step (1), in equipment, add linking agent, stir, the speed of stirring is 300 to turn again, and the suction in the equipment is-0.06MPa that the time of stirring is 5min;
(3), after the step (2), in equipment, add aerosil, stir, stirring velocity is 600 to turn again, and the suction in the equipment is-0.06MPa that the time of stirring is 10～30min;
(4), after the step (3), in equipment, add coupling agent, stir, the speed of stirring is 600 to turn again, the suction-0.06MPa in the equipment, and the time of stirring is 10min;
(5), after the step (4), in equipment, add catalyzer, stir, the speed of stirring is 600 to turn again, and the suction in the equipment is-0.06MPa that the time of stirring is 10min;
(6), pack after the discharging, place and carry out the transparency test after 72 hours, the testing method of transparency is: seal gum is made 5mm thickness film, be placed on after the curing on the blank sheet of paper of No. 5 words of the Song typeface, see through film and see word on the blank sheet of paper, being placed on the paper effect with the 5mm float glass equally is 1, is placed on the 10mm float glass that effect equally is 2 on the paper, the font of seeing some fuzzy be 3, distinguish that misknowing word content is 4, can only see that fuzzy word shadow is 5, word that can't see the back fully is 6.
Embodiment 2: a kind of high transparent self-vulcanizing silicon-ketone composition, carry out proportioning by following mass parts:
100 parts of hydroxyl endblocked polydimethylsiloxanes;
20 parts of alkyl-blocked polydimethylsiloxanes;
10 parts of aerosils;
0.00001 part of organic fluorescence agent;
20 parts of polyisobutene;
10 parts of linking agents;
1 part of coupling agent;
0.1 part of catalyzer.
The viscosity of described hydroxyl endblocked polydimethylsiloxane when temperature is 25 ℃ is 100Pa.S.
The specific surface area of described aerosil is 400m
2/ g.
Process with silazane or methyl chlorosilane on the surface of described aerosil.
Described organic fluorescence agent is colourless organic compound, and the organic fluorescence agent can absorbing wavelength be the ultraviolet ray of 350nm, and radiating wavelength is the bluish voilet fluorescence of 450nm.
Described organic fluorescence agent is the mixture of distyryl biphenyl class, coumarins;
Described coupling agent is the mixture of aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl trimethoxysilane;
Described catalyzer be dibutyl tin laurate, dibutyltin diacetate, Dibutyltin oxide, mixture.
Described polyisobutene is low-molecular weight polymer, and the polymerization degree of polyisobutene is 200, and the viscosity of polyisobutene is 1Pa.s.
Described linking agent is the mixture of methyltrimethoxy silane, vinyltrimethoxy silane, tetramethoxy-silicane, Union carbide A-162.
When described linking agent was methyl three (methyl isobutyl ketoxime base) silane, the molecular formula of methyl three (methyl isobutyl ketoxime base) silane was: C19H39N3SI03
A kind of preparation method of high transparent self-vulcanizing silicon-ketone composition, carry out according to the following steps:
(1), in the equipment that can vacuumize, disperse with brute force oar, adds hydroxyl endblocked polydimethylsiloxane, polyisobutene, organic fluorescence agent, stir, the speed that stirs is 500 to turn, and the suction in the equipment is-0.08MPa that the time of stirring is 20min;
(2), after the step (1), in equipment, add linking agent, stir, the speed of stirring is 700 to turn again, and the suction in the equipment is-0.08MPa that the time of stirring is 20min;
(3), after the step (2), in equipment, add aerosil, stir, stirring velocity is 800 to turn again, and the suction in the equipment is-0.08MPa that the time of stirring is 20min;
(4), after the step (3), in equipment, add coupling agent, stir, the speed of stirring is 800 to turn again, the suction-0.08MPa in the equipment, and the time of stirring is 15min;
(5), after the step (4), in equipment, add catalyzer, stir, the speed of stirring is 800 to turn again, and the suction in the equipment is-0.08MPa that the time of stirring is 15min;
(6), pack after the discharging, place and carry out the transparency test after 72 hours, the testing method of transparency is: seal gum is made 5mm thickness film, be placed on after the curing on the blank sheet of paper of No. 5 words of the Song typeface, see through film and see word on the blank sheet of paper, being placed on the paper effect with the 5mm float glass equally is 1, is placed on the 10mm float glass that effect equally is 2 on the paper, the font of seeing some fuzzy be 3, distinguish that misknowing word content is 4, can only see that fuzzy word shadow is 5, word that can't see the back fully is 6.
Embodiment 3: a kind of high transparent self-vulcanizing silicon-ketone composition is characterized in that carrying out proportioning by following mass parts:
100 parts of hydroxyl endblocked polydimethylsiloxanes;
50 parts of alkyl-blocked polydimethylsiloxanes;
20 parts of aerosils;
0.0001 part of organic fluorescence agent;
50 parts of polyisobutene;
20 parts of linking agents;
2 parts of coupling agents;
0.2 part of catalyzer.
The viscosity of described hydroxyl endblocked polydimethylsiloxane when temperature is 25 ℃ is 200Pa.S.
The specific surface area of described aerosil is 500m
2/ g.
Process with silazane or methyl chlorosilane on the surface of described aerosil.
Described organic fluorescence agent is colourless organic compound, and the organic fluorescence agent can absorbing wavelength be the ultraviolet ray of 400nm, and radiating wavelength is the bluish voilet fluorescence of 480nm.
Described organic fluorescence agent is the mixture of distyryl biphenyl class, coumarins, Phthalimide class fluorescent agent;
Described coupling agent is the mixture of aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl trimethoxysilane, N-β aminoethyl γ aminopropyl trimethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane;
Described catalyzer is the mixture of dibutyl tin laurate, dibutyltin diacetate, Dibutyltin oxide, ethyl-diacetyl-acetate diisopropoxy titanium.
Described polyisobutene is low-molecular weight polymer, and the polymerization degree of polyisobutene is 300, and the viscosity of polyisobutene is 2Pa.s.
Described linking agent is the mixture of methyltrimethoxy silane, vinyltrimethoxy silane, tetramethoxy-silicane, Union carbide A-162, methyl triacetoxysilane, vinyltriacetoxy silane, tetrem acyloxy silane, methyl tributanoximo silane, vinyl three ketoximinosilanes, phenyl tributanoximo silane, four Diacetylmonoxime base silanes, methyl three (methyl isobutyl ketoxime base) silane.
When described linking agent was methyl three (methyl isobutyl ketoxime base) silane, the molecular formula of methyl three (methyl isobutyl ketoxime base) silane was: C19H39N3SI03
A kind of preparation method of high transparent self-vulcanizing silicon-ketone composition, carry out according to the following steps:
(1), in the equipment that can vacuumize, disperse with brute force oar, adds hydroxyl endblocked polydimethylsiloxane, polyisobutene, organic fluorescence agent, stir, the speed that stirs is 1000 to turn, and the suction in the equipment is-0.1MPa that the time of stirring is 30min;
(2), after the step (1), in equipment, add linking agent, stir, the speed of stirring is 1000 to turn again, and the suction in the equipment is-0.1MPa that the time of stirring is 30min;
(3), after the step (2), in equipment, add aerosil, stir, stirring velocity is 1000 to turn again, and the suction in the equipment is-0.1MPa that the time of stirring is 30min;
(4), after the step (3), in equipment, add coupling agent, stir, the speed of stirring is 1000 to turn again, the suction-0.1MPa in the equipment, and the time of stirring is 20min;
(5), after the step (4), in equipment, add catalyzer, stir, the speed of stirring is 1000 to turn again, and the suction in the equipment is-0.1MPa that the time of stirring is 20min;
(6), pack after the discharging, place and carry out the transparency test after 72 hours, the testing method of transparency is: seal gum is made 5mm thickness film, be placed on after the curing on the blank sheet of paper of No. 5 words of the Song typeface, see through film and see word on the blank sheet of paper, being placed on the paper effect with the 5mm float glass equally is 1, is placed on the 10mm float glass that effect equally is 2 on the paper, the font of seeing some fuzzy be 3, distinguish that misknowing word content is 4, can only see that fuzzy word shadow is 5, word that can't see the back fully is 6.
Claims (10)
1. one kind high transparent self-vulcanizing silicon-ketone composition is characterized in that carrying out proportioning by following mass parts:
100 parts of hydroxyl endblocked polydimethylsiloxanes;
0～50 part of alkyl-blocked polydimethylsiloxane;
3～20 parts of aerosils;
0.000001～0.0001 part of organic fluorescence agent;
1～50 part of polyisobutene;
1～20 part of linking agent;
0.1～2 part of coupling agent;
0.01～0.2 part of catalyzer.
2. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1, it is characterized in that: the viscosity of described hydroxyl endblocked polydimethylsiloxane when temperature is 25 ℃ is 0.5～200Pa.S.
3. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1, it is characterized in that: the specific surface area of described aerosil is 300～500m
2/ g.
4. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1 is characterized in that: process with silazane or methyl chlorosilane on the surface of described aerosil.
5. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1, it is characterized in that: described organic fluorescence agent is colourless organic compound, the organic fluorescence agent can absorbing wavelength be the ultraviolet ray of 300～400nm, and radiating wavelength is the bluish voilet fluorescence of 420～480nm.
6. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1 is characterized in that: described organic fluorescence agent is one or more the mixture in distyryl biphenyl class, coumarins, the Phthalimide class fluorescent agent;
Described coupling agent is one or more the mixture in aminopropyl trimethoxysilane, aminopropyl triethoxysilane, aminopropyl trimethoxysilane, N-β aminoethyl γ aminopropyl trimethoxysilane, the 3-glycidyl ether oxygen base propyl trimethoxy silicane;
Described catalyzer is one or more the mixture in dibutyl tin laurate, dibutyltin diacetate, Dibutyltin oxide, the ethyl-diacetyl-acetate diisopropoxy titanium.
7. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1, it is characterized in that: described polyisobutene is low-molecular weight polymer, and the polymerization degree of polyisobutene is 3～300, and the viscosity of polyisobutene is 0.002～2Pa.s.
8. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1 is characterized in that: described linking agent is one or more the mixture in methyltrimethoxy silane, vinyltrimethoxy silane, tetramethoxy-silicane, Union carbide A-162, methyl triacetoxysilane, vinyltriacetoxy silane, tetrem acyloxy silane, methyl tributanoximo silane, vinyl three ketoximinosilanes, phenyl tributanoximo silane, four Diacetylmonoxime base silanes, methyl three (methyl isobutyl ketoxime base) silane.
9. a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 8, it is characterized in that: when described linking agent was methyl three (methyl isobutyl ketoxime base) silane, the molecular formula of methyl three (methyl isobutyl ketoxime base) silane was: C19H39N3SI03
?。
10. the preparation method of a kind of high transparent self-vulcanizing silicon-ketone composition according to claim 1 is characterized in that carrying out according to the following steps:
(1), in the equipment that can vacuumize, disperse with brute force oar, adds hydroxyl endblocked polydimethylsiloxane, polyisobutene, organic fluorescence agent, stir, the speed that stirs is 300～1000 to turn, suction in the equipment is-0.06～-0.1MPa, the time of stirring is 5～30min;
(2), after the step (1), in equipment, add linking agent, stir, the speed of stirring is 300～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 5～30min;
(3), after the step (2), in equipment, add aerosil, stir, stirring velocity is 600～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 10～30min;
(4), after the step (3), in equipment, add coupling agent, stir, the speed of stirring is 600～1000 to turn again, the suction in the equipment-0.06～-0.1MPa, the time of stirring is 10～20min;
(5), after the step (4), in equipment, add catalyzer, stir, the speed of stirring is 600～1000 to turn again, the suction in the equipment is-0.06～-0.1MPa, the time of stirring is 10～20min;
(6), pack after the discharging, place and carry out the transparency test after 72 hours, the testing method of transparency is: seal gum is made 5mm thickness film, be placed on after the curing on the blank sheet of paper of No. 5 words of the Song typeface, see through film and see word on the blank sheet of paper, being placed on the paper effect with the 5mm float glass equally is 1, is placed on the 10mm float glass that effect equally is 2 on the paper, the font of seeing some fuzzy be 3, distinguish that misknowing word content is 4, can only see that fuzzy word shadow is 5, word that can't see the back fully is 6.
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| CN103937443A (en) * | 2014-04-23 | 2014-07-23 | 浙江中天氟硅材料有限公司 | Fluorescent anti-fouling silicone sealant for filling seams of ceramic bricks and preparation method thereof |
| CN104497960A (en) * | 2014-12-23 | 2015-04-08 | 广东欧利雅化工有限公司 | Room-temperature curable flame-retardant silicone sealant and preparation method thereof |
| CN105603748A (en) * | 2016-01-11 | 2016-05-25 | 苏州迈塔斯芯片科技有限公司 | Hydrophobic and oileophobic finishing agent and preparation method thereof |
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| CN103937443B (en) * | 2014-04-23 | 2015-12-30 | 浙江中天氟硅材料有限公司 | Antifouling silicone sealant of fluorescence of a kind of ceramic tile joint filling and preparation method thereof |
| CN103937443A (en) * | 2014-04-23 | 2014-07-23 | 浙江中天氟硅材料有限公司 | Fluorescent anti-fouling silicone sealant for filling seams of ceramic bricks and preparation method thereof |
| CN104497960A (en) * | 2014-12-23 | 2015-04-08 | 广东欧利雅化工有限公司 | Room-temperature curable flame-retardant silicone sealant and preparation method thereof |
| CN107531908A (en) * | 2015-04-02 | 2018-01-02 | 波利默里克斯有限公司 | Fluorescence silicone elastomer, the method and purposes for synthesizing it |
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| CN105603748A (en) * | 2016-01-11 | 2016-05-25 | 苏州迈塔斯芯片科技有限公司 | Hydrophobic and oileophobic finishing agent and preparation method thereof |
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| CN108610635A (en) * | 2018-05-08 | 2018-10-02 | 山东大学 | A kind of organic luminescence from silicon method for producing elastomers |
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| CN108893091B (en) * | 2018-05-18 | 2020-12-25 | 江苏中南建设装饰有限公司 | Fluorescent sealant for curtain wall and preparation method thereof |
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Application publication date: 20130925 |