CN105086925A - Novel environment-friendly flame-retardant silicone sealant and preparation method thereof - Google Patents
Novel environment-friendly flame-retardant silicone sealant and preparation method thereof Download PDFInfo
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- CN105086925A CN105086925A CN201510524661.9A CN201510524661A CN105086925A CN 105086925 A CN105086925 A CN 105086925A CN 201510524661 A CN201510524661 A CN 201510524661A CN 105086925 A CN105086925 A CN 105086925A
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Abstract
The invention discloses a novel environment-friendly flame-retardant silicone sealant and a preparation method thereof. The novel environment-friendly flame-retardant silicone sealant comprises, by weight, 100 parts of alpha, omega-dihydroxy polymethylsiloxane, 1-50 parts of polymethylsiloxane, 5-150 parts of filler, 1-10 parts of phosphorous silicone flame retardant, 1-15 parts of crosslinking agent, 0.1-3 parts of catalyst and 0.5-4 parts of coupling agent. The dealcoholized flame-retardant silicone sealant is prepared by adopting a method of adding novel environment-friendly flame retardant, so that the problem that dealcoholized flame-retardant sealant products are low in flame retardance is solved, and the preparation method is simple; loss is low in the process of production, and the sealant is high in processing performance.
Description
Technical field
The present invention relates to a kind of flame-proof silicone sealant and preparation method thereof, belong to high molecule sealing materials field.
Background technology
Silicone sealant have excellent heatproof, weather-proof, anti-aging, do not chap, the feature such as antidetonation and protection against the tide, be widely used in building, electronic apparatus, automobile, field of aerospace.Along with the enhancing of people's security against fire consciousness, require more and more higher to the fire rating of seal gum.Although ordinary silicon ketone seal gum has certain flame retardant properties, its flame retardant properties still can not reach industry requirement.By adding fire retardant to improve product flame retardant properties in silicone sealant, become a kind of feasible effective means.
Additive flame retardant is as aluminium hydroxide, magnesium hydroxide, they are nontoxic, smokeless, cheap, but the particle diameter of aluminium hydroxide, magnesium hydrate powder affects larger on the flame retardant resistance of silicone sealant and fillibility, exist mixing uneven or reunite so that and polymkeric substance between bonding force poor, cause degradation problem under superpolymer performance.
Halogen flame has good flame retardant effect in seal gum, but not only discharges a large amount of smog during burning, also can discharge toxic substance, produces detrimentally affect to environment.
Phosphorus flame retardant and polysiloxane consistency bad, add in seal gum and can produce the problem such as layering, infiltration, affect its store and use.Therefore, phosphorus flame retardant uses less in seal gum.
Silicon-series five-retardant silicon fire-retardant agent domestic production kind and turnout all very little, use more silicone polymer to be a kind of polysiloxane polymer of transparent, thickness.As the silicone polymer of fire retardant, usually and one or more synergists using.Because silicon-series five-retardant is mostly smokelessly few malicious, combustion heat value is low, and flame propagation velocity is slow, and therefore receive the concern of people, its development potentiality and application prospect are very considerable.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency overcoming the problems referred to above, provides the improvement opportunity of a kind of flame retardant sealant and preparation method thereof.
Technical solution of the present invention
A kind of novel environment friendly flame-proof silicone sealant, by weight, comprises following component:
More preferably comprise following component:
Described phosphorus silicon fire retardant is that 9,10-dihydro-9-oxy is mixed phosphorus hydrogen bond active in phenanthrene-10-oxide compound (DOPO) derivative and the siloxanes generation addition reaction containing two carbon-carbon double bonds and the fire retardant that generates, and the structural formula of this fire retardant is as follows:
Wherein, R
1, R
2, R
3, R
4, the alkyl that C1-C5 is selected from, the alkoxyl group of C1-C5, aryl, aryloxy; R
5with R
6for the alkylidene group of C0-C5; R
7-R
14be selected from hydrogen atom, the alkyl of C1-C5, nitro, the alkoxyl group of C1-C5, aryl, aryloxy; N is 1-10.
Described α, alpha, omega-dihydroxy polysiloxane viscosity 25 DEG C time is 16000 ~ 80000mPa/s.
Described polydimethylsiloxane viscosity 25 DEG C time is 50 ~ 1000mPa/s.
Described filler is at least one in gas-phase silica, nano-calcium carbonate, silicon powder, quartzite and diatomite, be preferably nano-calcium carbonate and gas-phase silica, and the weight ratio of nano-calcium carbonate and gas-phase silica is 15:1.
Described linking agent is at least one in tetraethoxy, methyltrimethoxy silane, Union carbide A-162 and vinyltriethoxysilane, is preferably Union carbide A-162.
Described catalyzer be dibutyl tin laurate, dibutyltin diacetate, butyl (tetra) titanate, at least one, be preferably dibutyltin diacetate.
Described coupling agent is γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicon, N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silicon and at least one in two (γ-trimethoxy-silylpropyl) amine, be preferably two (γ-trimethoxy-silylpropyl) amine.
The preparation method of described novel environment friendly flame-proof silicone sealant, comprises the following steps:
By α, alpha, omega-dihydroxy polysiloxane 100 parts, polydimethylsiloxane 1 ~ 50 part, filler 5 ~ 150 parts, novel environment friendly fire retardant 1 ~ 10 part, linking agent 1 ~ 15 part, catalyzer 0.1 ~ 3 part, coupling agent 0.5 ~ 4 part, add in planetary mixer, vacuum tightness is-0.1 ~-0.09, and rotating speed is discharging after stirring 2 ~ 6h under the condition of 12 ~ 50rmp, can obtain silicone sealant.
The invention has the beneficial effects as follows: the present invention adopts α, polymkeric substance based on alpha, omega-dihydroxy polysiloxane, preparing Dealcoholization type silicone sealant by adding the auxiliary agents such as fire retardant.When seal gum is prepared, first novel environment friendly fire retardant is mixed with 107 glue and make base-material, then add the auxiliary agents such as polydimethylsiloxane, filler, linking agent, catalyzer and be mixed with seal gum, prepared seal gum in use has the type of resistance to combustion and self-extinguishing type, flame retardant rating can reach V0 level, has the advantage of low toxicity, pollution-free, the good stable storing of cementability.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
Press α with each component described in following table 1 respectively, alpha, omega-dihydroxy polysiloxane, polydimethylsiloxane, gas-phase silica, two [(6-oxygen-6-hydrogen-dibenzo-(c, e) (1,2)-own the ring of oxygen phospha-6-ketone)-ethyl]-siloxanes adds in planetary mixer, vacuum tightness is-0.1 ~-0.09, rotating speed is stir 2-6h under the condition of 12 ~ 50rmp, by KH550, tetraethoxy after mixing, di lauric dibutyl rubber tin adds wherein, discharging after 10 ~ 20min, can obtain silicone sealant.Then test various performance, product test the results are shown in Table 2.
Embodiment 2
By the method repeating embodiment 1 with each component concentration described in following table 1, but fire retardant two [(6-oxygen-6-hydrogen-dibenzo-(c, e) (1, 2)-own the ring of oxygen phospha-6-ketone)-propyl group] the alternative two [(6-oxygen-6-hydrogen-dibenzo-(c of-siloxanes, e) (1, 2)-own the ring of oxygen phospha-6-ketone)-ethyl]-siloxanes, filler surface substitutes gas-phase silica through stearic acid modified nano-calcium carbonate, linking agent methyltrimethoxy silane substitutes tetraethoxy, coupling agent KH560 substitutes KH550, catalyzer butyl (tetra) titanate substitutes di lauric dibutyl rubber tin.Product test the results are shown in Table 2.
Embodiment 3
By the method repeating embodiment 1 with each component concentration described in following table 1, but filler active nano-calcium carbonate and gas-phase silica (wherein the weight ratio of active nano-calcium carbonate and gas-phase silica is 15:1) composite use substitute and are used alone gas-phase silica, linking agent Union carbide A-162 substitutes tetraethoxy, catalyzer dibutyltin diacetate substitutes di lauric dibutyl rubber tin, coupling agent KH170 substitutes KH550, and product test the results are shown in Table 2.
Embodiment 4
By the method repeating embodiment 1 with each component concentration described in following table 1, but filler silicon powder and gas-phase silica (wherein the weight ratio of silicon powder and gas-phase silica is 1:1) composite use substitute and are used alone gas-phase silica, linking agent vinyltriethoxysilane substitutes tetraethoxy, and product test the results are shown in Table 2.
Embodiment 5
By the method repeating embodiment 1 with each component concentration described in following table 1, but filler active nano-calcium carbonate and silicon powder (wherein the weight ratio of active nano-calcium carbonate and silicon powder is 6:1) composite use substitute gas-phase silica, and product test the results are shown in Table 2.
Comparative example
By the method repeating embodiment 1 with each component concentration described in following table 1, material therefor is consistent with case study on implementation 1.Product test the results are shown in Table 2.
Claims (10)
1. a novel environment friendly flame-proof silicone sealant, is characterized in that, by weight, comprises following component:
2. novel environment friendly flame-proof silicone sealant according to claim 1, is characterized in that, by weight, comprises following component:
3. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, it is characterized in that, described phosphorus silicon fire retardant is 9,10-dihydro-9-oxy is mixed phosphorus hydrogen bond active in phenanthrene-10-oxide compound (DOPO) derivative and the siloxanes generation addition reaction containing two carbon-carbon double bonds and the fire retardant that generates, and the structural formula of this fire retardant is as follows:
Wherein, R
1, R
2, R
3, R
4, the alkyl that C1-C5 is selected from, the alkoxyl group of C1-C5, aryl, aryloxy; R
5with R
6for the alkylidene group of C0-C5; R
7-R
14be selected from hydrogen atom, the alkyl of C1-C5, nitro, the alkoxyl group of C1-C5, aryl, aryloxy; N is 1-10.
4. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, is characterized in that, described α, and alpha, omega-dihydroxy polysiloxane viscosity 25 DEG C time is 16000 ~ 80000mPa/s.
5. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, is characterized in that, described polydimethylsiloxane viscosity 25 DEG C time is 50 ~ 1000mPa/s.
6. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, it is characterized in that, described filler is at least one in gas-phase silica, nano-calcium carbonate, silicon powder, quartzite and diatomite, be preferably nano-calcium carbonate and gas-phase silica, and the weight ratio of nano-calcium carbonate and gas-phase silica is 15:1.
7. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, it is characterized in that, described linking agent is at least one in tetraethoxy, methyltrimethoxy silane, Union carbide A-162 and vinyltriethoxysilane, is preferably Union carbide A-162.
8. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, is characterized in that, described catalyzer be dibutyl tin laurate, dibutyltin diacetate, butyl (tetra) titanate, at least one, be preferably dibutyltin diacetate.
9. novel environment friendly flame-proof silicone sealant according to claim 1 and 2, it is characterized in that, described coupling agent is γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicon, N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silicon and at least one in two (γ-trimethoxy-silylpropyl) amine, be preferably two (γ-trimethoxy-silylpropyl) amine.
10. the preparation method of the novel environment friendly flame-proof silicone sealant described in any one of claim 1-9, it is characterized in that, comprise the following steps: by α, alpha, omega-dihydroxy polysiloxane 100 parts, polydimethylsiloxane 1 ~ 50 part, filler 5 ~ 150 parts, novel environment friendly fire retardant 1 ~ 10 part, linking agent 1 ~ 15 part, catalyzer 0.1 ~ 3 part, coupling agent 0.5 ~ 4 part, add in planetary mixer, vacuum tightness is-0.1 ~-0.09, and rotating speed is discharging after stirring 2 ~ 6h under the condition of 12 ~ 50rmp, can obtain silicone sealant.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105440480A (en) * | 2015-12-10 | 2016-03-30 | 无锡普瑞腾传动机械有限公司 | Organic silicon sealant for automotive windscreen |
| CN107011661A (en) * | 2017-03-14 | 2017-08-04 | 清华大学 | Feedstock composition, quasi-iso static pressing soft mode and its manufacture method for manufacturing quasi-iso static pressing soft mode |
| CN108795367A (en) * | 2018-06-28 | 2018-11-13 | 芜湖市棠华建材科技有限公司 | Neutral room temperature sealing silicone sulfide glue |
| CN108977166A (en) * | 2018-06-28 | 2018-12-11 | 芜湖市棠华建材科技有限公司 | A kind of silicone sealant and preparation method thereof |
| CN109810670A (en) * | 2019-01-30 | 2019-05-28 | 温州包鹿新材料有限公司 | A kind of bi-component fire prevention silicone sealant and preparation method thereof |
| CN115851219A (en) * | 2023-01-05 | 2023-03-28 | 山东元腾新材料科技有限公司 | Silicone flame-retardant sealant for construction |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438289A (en) * | 2003-03-06 | 2003-08-27 | 成都硅宝科技实业有限责任公司 | Neutral silicone fire-retardent sealing glue and its preparing method |
| CN1687288A (en) * | 2005-04-13 | 2005-10-26 | 成都硅宝科技实业有限责任公司 | Flameproofing silicone structure sealant and mfg. method thereof |
| CN1865383A (en) * | 2006-06-23 | 2006-11-22 | 陈世龙 | Flame-proof silicone sealant for electronics and its production method |
| CN101445520A (en) * | 2007-11-26 | 2009-06-03 | 中国科学院化学研究所 | Phosphoric organic silicon compound, preparation method and application thereof |
| CN101629063A (en) * | 2009-08-24 | 2010-01-20 | 陈世龙 | Expanding type flame-resistant silicone sealant and preparation method thereof |
| CN101747859A (en) * | 2010-01-29 | 2010-06-23 | 浙江凌志精细化工有限公司 | Silicone fireproof sealant for construction and preparation method thereof |
| CN103160239A (en) * | 2011-12-19 | 2013-06-19 | 广州市白云化工实业有限公司 | High-displacement-ability silicone fire-proof sealing glue and manufacturing method of the same |
-
2015
- 2015-08-25 CN CN201510524661.9A patent/CN105086925B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1438289A (en) * | 2003-03-06 | 2003-08-27 | 成都硅宝科技实业有限责任公司 | Neutral silicone fire-retardent sealing glue and its preparing method |
| CN1687288A (en) * | 2005-04-13 | 2005-10-26 | 成都硅宝科技实业有限责任公司 | Flameproofing silicone structure sealant and mfg. method thereof |
| CN1865383A (en) * | 2006-06-23 | 2006-11-22 | 陈世龙 | Flame-proof silicone sealant for electronics and its production method |
| CN101445520A (en) * | 2007-11-26 | 2009-06-03 | 中国科学院化学研究所 | Phosphoric organic silicon compound, preparation method and application thereof |
| CN101629063A (en) * | 2009-08-24 | 2010-01-20 | 陈世龙 | Expanding type flame-resistant silicone sealant and preparation method thereof |
| CN101747859A (en) * | 2010-01-29 | 2010-06-23 | 浙江凌志精细化工有限公司 | Silicone fireproof sealant for construction and preparation method thereof |
| CN103160239A (en) * | 2011-12-19 | 2013-06-19 | 广州市白云化工实业有限公司 | High-displacement-ability silicone fire-proof sealing glue and manufacturing method of the same |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105440480A (en) * | 2015-12-10 | 2016-03-30 | 无锡普瑞腾传动机械有限公司 | Organic silicon sealant for automotive windscreen |
| CN107011661A (en) * | 2017-03-14 | 2017-08-04 | 清华大学 | Feedstock composition, quasi-iso static pressing soft mode and its manufacture method for manufacturing quasi-iso static pressing soft mode |
| CN108795367A (en) * | 2018-06-28 | 2018-11-13 | 芜湖市棠华建材科技有限公司 | Neutral room temperature sealing silicone sulfide glue |
| CN108977166A (en) * | 2018-06-28 | 2018-12-11 | 芜湖市棠华建材科技有限公司 | A kind of silicone sealant and preparation method thereof |
| CN109810670A (en) * | 2019-01-30 | 2019-05-28 | 温州包鹿新材料有限公司 | A kind of bi-component fire prevention silicone sealant and preparation method thereof |
| CN109810670B (en) * | 2019-01-30 | 2022-02-01 | 江苏赛欧信越消泡剂有限公司 | Bi-component fireproof silicone sealant and preparation method thereof |
| CN115851219A (en) * | 2023-01-05 | 2023-03-28 | 山东元腾新材料科技有限公司 | Silicone flame-retardant sealant for construction |
| CN115851219B (en) * | 2023-01-05 | 2023-11-07 | 山东元腾新材料科技有限公司 | Silicone flame-retardant sealant for building |
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Address after: 443007 No. 66-2 Ting Ting Road, Ting Ting District, Yichang, Hubei Patentee after: Hubei Xingrui silicon material Co., Ltd. Address before: 443006 No. 29 Changjiang Road, Ting Ting District, Yichang, Hubei Patentee before: HUBEI XINGRUI CHEMICAL CO., LTD. |