CN101760172A - Single-component dealcoholization-type organic silicon sealant - Google Patents
Single-component dealcoholization-type organic silicon sealant Download PDFInfo
- Publication number
- CN101760172A CN101760172A CN200810236984A CN200810236984A CN101760172A CN 101760172 A CN101760172 A CN 101760172A CN 200810236984 A CN200810236984 A CN 200810236984A CN 200810236984 A CN200810236984 A CN 200810236984A CN 101760172 A CN101760172 A CN 101760172A
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- organic silicon
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- titanate
- component dealcoholization
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Abstract
The invention relates to a single-component dealcoholization-type organic silicon sealant which belongs to the technical field of single-component organic silicon sealant and mainly solves the problem of poor adhesiveness and storage stability of the traditional sealant. The single-component dealcoholization-type organic silicon sealant comprises the following components in percentage by weight: 30-70 wt% of hydroxy-terminated poly dimethylsiloxane polymer, 15-50 wt% of nano-scale calcium carbonate, 2-10 wt% of alkoxy silane crosslinker, 0.1-3 wt% of titanate chelate catalyst, 1-5 wt% of thixotropic agent, 0.05-2 wt% of titanate catalyst, 0.1-2 wt% of coupling agent and 0.5- 5wt% of silicone oil plasticizer. The invention has favorable mechanical performance and excellent adhesiveness as well as double-85 resistant performance, has simple construction process and is widely used for splicing and sealing solar modules in the solar photovoltaic industry.
Description
Technical field
The invention belongs to single-component organic silicon sealing agent technical field; be specifically related to ((85 ℃ of a kind of anti-" two 85 " performances; 85%RH) * 1000h after index request such as tensile strength, elongation, hardness), shelf-stable, seal gum excellent in adhesion; be directly used in the bonding of assemblies such as sealing of solar photovoltaic assembly frame and terminal box; effectively not contaminated, the oxidation of protection silicon wafer, bonding, the fixing seal of electronics, electric parts and the packaging protection of insulation, outdoor LED display and backlight.Have high strength, high adhesion, and guarantee to be glued not xanthochromia of assembly composite membrane.The present invention is mainly used in the bonding of photovoltaic industry solar components and sealing.
Background technology
U.S. Pat 4687829 adopts the catalyzer of end alkoxy group silicon ethylene group to improve package stability and cementability, but effect is undesirable.Use terminal trimethoxy siloxane to be basic glue among the Chinese patent CN10101236A, titanate chelate improves its stability and cementability as the system of catalyzer, but the structure adhering and sealing that it is mainly used in various curtain walls and metal construction engineering can not be directly used in the adhering and sealing of solar components.The patent that dealcoholizing-type silica gel is relevant is consulted, the report of anti-" two 85 " performance is not also arranged.
Summary of the invention
The objective of the invention is provides a kind of single-component room temperature vulcanized dealcoholizing-type organic silicon sealant with distinguishing features such as adhesiveproperties excellence, shelf-stable, anti-" two 85 " excellent performances at the deficiency that has dealcoholizing-type silica gel technology now.
Purpose of the present invention is realized that by following technical measures wherein said starting material umber is mass fraction except that specified otherwise.
The prescription of single-component room temperature vulcanized dealcoholizing-type organic silicon sealant consists of:
(a) 30%～70%Wt hydroxyl-terminated injecting two methyl siloxane polymkeric substance;
(b) 15%～50%Wt nanometer grade calcium carbonate;
(c) 2%～10%Wt makes alkoxy silane cross linked dose of two silicone cross-linked solidified of hydroxyl when moisture exists;
(d) 0.1%～3%Wt titanate chelate class catalyzer;
(e) 1%～5%Wt thixotropic agent;
(f) 0.05%～2%Wt titanate ester catalyzer;
(g) 0.1%～2%Wt coupling agent;
(h) 0.5%～5%Wt silicone oil softening agent.
Wherein hydroxyl-terminated injecting two methyl siloxane polymericular weight Mn is 4200～44, and between 000, average viscosity is 100～20 in the time of 25 ℃, 000cps.
Nanometer grade calcium carbonate is the nanometer grade calcium carbonate through hydrophobic treatment, and median size is 0.05um, has regular crystalline form and size distribution, surface active, crystal habit controlling features accurately efficiently.
Linking agent is R for one or more have general formula
1 4-nSi (OR
2)
nSiloxanes, wherein R is saturated, unsaturated straight or branched alkyl of 1～4 carbon atom, n is 0～4, R
1And R
2Saturated, the unsaturated straight or branched alkyl that have 1～4 carbon atom independently of each other.
Thixotropic agent is the gas-phase silica of different specific surface areas.
Titanate chelate class catalyzer is methyl aceto acetate-isopropyl titanate inner complex, under the condition of wetly existence, can quicken the curing of composition.
Silane coupling agent is aminopropyl triethoxysilane, glycidoxypropyltrime,hoxysilane, aminoethyl aminopropyl triethoxysilane or its mixture.
The titanate ester catalyzer is tetrabutyl titanate, metatitanic acid third different ester or the isopropyl titanate, under the condition of wetly existence, can quicken the fast setting of composition.
Softening agent is the polydimethylsiloxane of methyl blocking, and viscosity is 100～20000cps under the standard conditions.
The preparation technology of single-component room temperature vulcanized dealcoholizing-type organic silicon sealant is as follows:
At room temperature, with hydroxyl-terminated injecting two methyl siloxane polymkeric substance 30%～70%, 15%～50% pearl filler, alkoxy silane cross linked dose of 2%～10%Wt, 0.1%～3% titanate chelate class catalyzer, 1%～5% thixotropic agent, 0.05%～2% titanate ester catalyzer, 0.1%～2% coupling agent, 0.5～5% silicone oil softening agent, add in the high speed dispersor, wherein catalyzer divides two stages to add, at isolated moisture (vapour), vacuum tightness stirs 120～150min to being uniformly dispersed under the condition of-0.08～0.1MPa, can obtain single-component room temperature vulcanized dealcoholizing-type organic silicon sealant, installs in following minute to seal in the packing tube at the state that completely cuts off moisture (vapour) to get final product.
Performance test requirement of the present invention and method are as follows:
The cementability test, material is two kinds of stainless steel substrates and aluminium test pieces, glue is applied to by sticking metal testing plate surface, bondline thickness control 1.5 ± 0.5mm, then with two test pieces to folded, bond area is 20mm * 10mm, makes bonding plane pressurized 0.05～0.1Mpa, solidify after 7 days and take out, measure shearing resistance according to GB/T7124.
Hardness test is undertaken by GB/T531-1999 standard code method.
Tensile strength and test of elongation rate place mould on the foil paper, with the glue rifle seal gum are injected in the mould.Flatten, unnecessary seal gum is scraped off, mold removal from the foil paper.Bondline thickness is 2.5～3.0mm.Under the condition of temperature (23 ± 5) ℃, relative humidity (55 ± 5) %, solidify 7d, take out film, be cut into the mute tinkling of pieces of jade shape of specified dimension.With the draw speed of 500mm/min, test normal temperature tensile strength and normal temperature elongation.
The tear strength test places mould on the foil paper, with the glue rifle seal gum glue is injected in the mould.Flatten, unnecessary seal gum is scraped off, mold removal from the foil paper.Bondline thickness is 2.5～3.0mm.Under the condition of temperature (23 ± 5) ℃, relative humidity (55 ± 5) %, solidify 7d, take out film, be cut into the specified dimension shape.With the draw speed of 500mm/min, test normal temperature tear strength.
Anti-" two 85 " performance test is positioned over the film of self-vulcanizing 7d in the climatic chamber, and temperature is made as 85 ℃, and humidity is made as 85%RH, takes out behind the 1000h and is cooled to room temperature, is cut into the dumb-bell shape of specified dimension.With the draw speed of 500mm/min, test tensile strength, elongation and hardness after its anti-" two 85 ", and observe it and have or not the xanthochromia phenomenon.
The The performance test results of single-component dealcoholization-type organic silicon sealant sees attached list 1.
It is that the nanometer grade calcium carbonate of 0.05um is a reinforced filling that the present invention adopts median size, titanate chelate and titanic acid ester are catalyzer, catalyzer adds in two steps, this is the main difference part of the present invention and other inventions, because the titanate chelate activity is less, slowly promote pre-reaction earlier, alleviated viscosity peak phenomenon, add active high titanate catalyst again, can improve cross-linking density, thereby raising intensity has been avoided the material vigorous reaction and the phenomenon of thickening, has suppressed the phenomenon on viscosity peak.And the glue of the preparation according to the present invention has excellent anti-" two 85 " performance, is mainly used in the bonding of photovoltaic industry solar components and sealing, and this is the present invention and the main difference of other dealcoholizing-type silica gel patent.
The present invention has following advantage:
1. the technology of the rational proportion of titanate chelate and two kinds of catalyzer of titanic acid ester and interpolation has in two steps suppressed the phenomenon of material thickening in the sealing agent production process, has reduced the requirement of production technique, has also improved cross-linking density; Adopting nanometer grade calcium carbonate simultaneously is reinforced filling, and good strengthening action is arranged; Comprehensively the two effect has improved anti-" two 85 " performance, every mechanical property keeps fine in " two 85 " test back, not flavescence of film, be not clamminess, do not feel like jelly, can be directly used in the bonding of the various assemblies of photovoltaic industry and sealing, in solidification process, base material is not had corrosion, and construction technology is easy, and is environmentally friendly.
2. adopt aminopropyl triethoxysilane, glycidoxypropyltrime,hoxysilane, aminoethyl aminopropyl triethoxysilane as coupling agent, improved the bonding strength of single-component dealcoholization-type organic silicon sealant, and collapse mode is cohesive failure to base material.
Embodiment
The following example will be introduced the present invention more in detail, but the present invention is not limited to this.
Embodiment 1
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 60%Wt
Nanometer grade calcium carbonate 26%Wt
Methyltrimethoxy silane 9%Wt
Methyl aceto acetate-isopropyl titanate inner complex 0.2%Wt
Gas-phase silica 2%Wt
Tetrabutyl titanate 2%Wt
Aminopropyl triethoxysilane 0.1%Wt
Glycidoxypropyltrime,hoxysilane 0.1%Wt
Dimethyl siloxane 0.6%Wt
Embodiment 2
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 45%Wt
Nanometer grade calcium carbonate 35%Wt
Union carbide A-162 7%Wt
Methyl aceto acetate-isopropyl titanate inner complex 0.2%Wt
Gas-phase silica 5%Wt
Tetrabutyl titanate 0.8%Wt
Aminopropyl triethoxysilane 1%Wt
Glycidoxypropyltrime,hoxysilane 1%Wt
Dimethyl siloxane 5%Wt
Embodiment 3
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 53%Wt
Nanometer grade calcium carbonate 30%Wt
Vinyltrimethoxy silane 6%Wt
Methyl aceto acetate-isopropyl titanate inner complex 2%Wt
Gas-phase silica 3%Wt
The metatitanic acid third different ester 0.2%Wt
Aminopropyl triethoxysilane 0.4%Wt
Glycidoxypropyltrime,hoxysilane 0.4%Wt
Dimethyl siloxane 5%Wt
Embodiment 4
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 61.2%Wt
Nanometer grade calcium carbonate 30%Wt
Methyltrimethoxy silane 4%Wt
Methyl aceto acetate-isopropyl titanate inner complex 1%Wt
Gas-phase silica 2%Wt
Isopropyl titanate 1%Wt
Aminoethyl aminopropyl triethoxysilane 0.2%Wt
Glycidoxypropyltrime,hoxysilane 0.1%Wt
Dimethyl siloxane 0.5%Wt
Embodiment 5
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 45%Wt
Nanometer grade calcium carbonate 42.7%Wt
Vinyltrimethoxy silane 2%Wt
Methyl aceto acetate-isopropyl titanate inner complex 0.8%Wt
Gas-phase silica 5%Wt
Tetrabutyl titanate 1.5%Wt
Tetrabutyl titanate 1%Wt
Aminoethyl aminopropyl triethoxysilane 0.5%Wt
Glycidoxypropyltrime,hoxysilane 0.5%Wt
Dimethyl siloxane 1%Wt
Comparative example 1
Hydroxyl-terminated injecting two methyl siloxane polymkeric substance 65.5%Wt
Import nanometer grade calcium carbonate 15%Wt
Methyltrimethoxy silane 5%Wt
Methyl aceto acetate-isopropyl titanate inner complex 3%Wt
Gas-phase silica 5%Wt
Tetrabutyl titanate 2%Wt
Aminoethyl aminopropyl triethoxysilane 0.2%Wt
Glycidoxypropyltrime,hoxysilane 0.3%Wt
Dimethyl siloxane 4%Wt
Subordinate list 1
The invention provides a kind of single-component room temperature vulcanized dealcoholized type organic silicon sealant; the sealing agent uses the nanometer grade calcium carbonate through hydrophobic treatment to be reinforced filling; being used titanate chelate and titanate esters is catalyst; after the technology of adjusting suitable ratio and adding in two steps; its glue has the adhesive property excellence; stable storage; the distinguishing features such as anti-" two 85 " excellent performance; be used for the bonding of the assemblies such as the sealing of solar photovoltaic assembly frame and terminal box; effectively the protection silicon wafer is not contaminated; oxidation, electronics; electric parts bonding; fixing seal and insulation; the packaging protection of outdoor LED display screen and backlight.
Claims (9)
1. single-component dealcoholization-type organic silicon sealant is characterized in that its composition comprises:
(a) 30%～70%Wt hydroxyl-terminated injecting two methyl siloxane polymkeric substance;
(b) 15%～50%Wt nanometer grade calcium carbonate;
(c) 2%～10%Wt makes alkoxy silane cross linked dose of two silicone cross-linked solidified of hydroxyl when moisture exists;
(d) 0.1%～3%Wt titanate chelate class catalyzer;
(e) 1%～5%Wt thixotropic agent;
(f) 0.05%～2%Wt titanate ester catalyzer;
(g) 0.1%～2%Wt coupling agent;
(h) 0.5%～5%Wt silicone oil softening agent.
2. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: the molecular weight Mn of described hydroxyl-terminated injecting two methyl siloxane polymkeric substance is 4200～44, and between 000, average viscosity is 100～20 in the time of 25 ℃, 000cps.
3. single-component dealcoholization-type organic silicon sealant according to claim 1, it is characterized in that: described nanometer grade calcium carbonate is the nanometer grade calcium carbonate through hydrophobic treatment, median size is 0.05um, has regular crystalline form and size distribution, surface active, crystal habit controlling features accurately efficiently.
4. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: described alkoxy silane cross linked dose is R for having general formula
1 4-nSi (OR
2)
nSiloxanes, wherein R is saturated, unsaturated straight or branched alkyl of 1～4 carbon atom, n is 0～4, R
1And R
2Saturated, the unsaturated straight or branched alkyl that have 1～4 carbon atom independently of each other.
5. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: described titanate chelate class catalyzer is methyl aceto acetate-isopropyl titanate inner complex, under the condition of wetly existence, can quicken the curing of composition.
6. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: described thixotropic agent is the gas-phase silica of different specific surface areas.
7. single-component dealcoholization-type organic silicon sealant according to claim 1, it is characterized in that: described titanate ester catalyzer is tetrabutyl titanate, metatitanic acid third different ester or the isopropyl titanate, under the condition of wetly existence, can quicken the fast setting of composition.
8. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: described coupling agent is aminopropyl triethoxysilane, glycidoxypropyltrime,hoxysilane, aminoethyl aminopropyl triethoxysilane or its mixture.
9. single-component dealcoholization-type organic silicon sealant according to claim 1 is characterized in that: described softening agent is a dimethyl siloxane, and viscosity is 100～20000cps under the standard conditions.
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| CN200810236984A CN101760172A (en) | 2008-12-24 | 2008-12-24 | Single-component dealcoholization-type organic silicon sealant |
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|---|---|---|---|
| CN200810236984A CN101760172A (en) | 2008-12-24 | 2008-12-24 | Single-component dealcoholization-type organic silicon sealant |
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| CN102093721A (en) * | 2010-09-14 | 2011-06-15 | 抚顺哥俩好化学有限公司 | Single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and preparation method thereof |
| CN102146208A (en) * | 2011-01-26 | 2011-08-10 | 广州市高士实业有限公司 | Method for preparing transparent dealcoholized single-component room temperature vulcanized silicone rubber |
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| CN102408868A (en) * | 2010-09-20 | 2012-04-11 | 广州市回天精细化工有限公司 | Fast deep cured single-component dealcoholization type organic silicon casting glue and preparation method |
| CN102146208A (en) * | 2011-01-26 | 2011-08-10 | 广州市高士实业有限公司 | Method for preparing transparent dealcoholized single-component room temperature vulcanized silicone rubber |
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| CN110776871A (en) * | 2019-10-22 | 2020-02-11 | 深圳市美信分析技术有限公司 | Room-temperature dealcoholized silicone adhesive and preparation method thereof |
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Application publication date: 20100630 |