CN104099060A - Two-composition fireproof silicone sealant - Google Patents
Two-composition fireproof silicone sealant Download PDFInfo
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- CN104099060A CN104099060A CN201310115381.3A CN201310115381A CN104099060A CN 104099060 A CN104099060 A CN 104099060A CN 201310115381 A CN201310115381 A CN 201310115381A CN 104099060 A CN104099060 A CN 104099060A
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Abstract
The invention relates to a preparation method for a two-composition fireproof silicone sealant. The method comprises the following steps: 1) adding 100 parts by weight of alpha, omega-dihydroxy polysiloxanes and 10-60 parts by weight of a filler/flame retardant composite composition into a kneading machine, performing mixing dewatering at 110-140 DEG C, under the vacuum degree of 0.06-0.1 MPa for 30-360 min, and cooling to obtain a base material; and 2) successively adding 0.5-2 parts by weight of a cross-linking agent, 0.1-0.5 part by weight of a catalyst and 5-20 parts by weight of methyl silicone oil into a high-speed dispersion machine, mixing with the above base material at room temperature under the vacuum degree of 0.06-0.1 MPa with the rotation speed of 600 rpm for 30-120 min, so as to obtain the fireproof silicone sealant. The silicone sealant prepared by using the method is capable of providing excellent flame retardation performance without reducing the mechanical properties of the system.
Description
Technical field
The present invention relates to silicone sealant field, particularly a kind of pair of component fire prevention silicone sealant.
Background technology
Along with the continuous expansion of macromolecular material Application Areas, organosilicon material application is more and more extensive, and range of application has contained nearly all industrial circle, is paid much attention to.The macromolecular material as a class with excellent properties is used widely, and is described as the monosodium glutamate of modern industry.
Organosilicon macromolecule is in molecular structure, to contain the polymkeric substance that connects organic radical on elemental silicon and Siliciumatom, is conventionally divided into four classes: silicone oil, silicone resin, silicon rubber, silane coupling agent are ridiculed.Organic silicon sealant is a kind of of silicon rubber.Organic silicon sealant is added the components such as weighting agent, strengthening agent, coupling agent, catalyzer to process by organosilicon polymer.Its main chain consists of siloxane bond, and side chain combines from different organic groups by Siliciumatom, forms a series of products.It has the performance of many uniquenesses, as high-and low-temperature resistance, and weather-proof, ageing-resistant, resistance to ozone, hydrophobic, difficult combustion, nontoxic, physiology inertia, good electrical insulating property, the outstanding advantages such as surfactivity.These performances are that other organic polymer materials can not compare and substitute, thereby be widely used at aspects such as aerospace, electric, chemical industry, machinery, building, communications and transportation, health care, agricultural and people's daily lifes, become brand-new material important in national economy.
Also there are many weakness in organosilicon material, such as intensity is low, inflammable, does not possess anti-flaming function etc., limited its application.Along with China's modern industry, particularly the high speed development of aerospace cause, more and more harsher to material performance requirement.Safety of China production situation is more and more serious at present, and the safety requirements of material is improved constantly.Organic silicon sealant is carried out to modification, improve constantly its over-all properties, particularly by adding good fire retardant, improve its flame retardant properties, significant, also there are wide market outlook.
Fire retardant is divided into inorganic system, organic system (brominated system, organophosphorus system, chlorine system) and other, the maximum organic fire-retardant of usage quantity is bromine compounds at present, but while burning due to bromine compounds, easily produce the carcinogenic substances such as Dioxins, for environmental protection, consider, the developed country such as American-European-Japanese is just starting to gradually reduce the usage quantity of bromine compounds fire retardant, and most promising replacement product are inorganic combustion inhibitors.How fire retardant is evenly added in organic materials, it is the important factor that determines fire retardant usage quantity, because most of inorganic combustion inhibitor is as larger in surface polarities such as aluminium hydroxide, magnesium hydroxides, machining property is bad, must select the magnesium hydroxide of appropriate particle size, suitable specific surface to carry out surface modification.
In prior art, with α, alpha, omega-dihydroxy polydimethyl siloxane is base glue, and thermal silica is filler, through the inorganic combustion inhibitor of surface modification, prepares single-component de-alcoholized fire-retardant self cure (RTV) silicone encapsulant.But when improving flame retardant properties, the mechanical property of system reduces greatly, has a strong impact on the range of application of organosilicon sealant.
Summary of the invention
The object of this invention is to provide a kind of pair of component flame-proof silicone sealant and preparation method thereof, it can provide excellent fire resistance the silicone sealant that the method is prepared, and does not reduce the mechanical property of system simultaneously.
Of the present invention pair of component fire prevention silicone sealant is comprised of A component and B component, and described A component is comprised of the component of following weight parts:
α, alpha, omega-dihydroxy polysiloxane 100 weight parts
Polydimethylsiloxane 15-80 weight part
Filler 50-150 weight part
Silane coupling agent 0.2-2 weight part
Water glass curing agent 0.1-10 weight part
Described B component is comprised of the component of following weight parts:
Water glass 5-50 weight part
Linking agent 0.5-10 weight part
Silane coupling agent 0.2-2 weight part
Chainextender 0.05-1 weight part
Catalyzer 0.1-5 weight part
in A component:
Described α, alpha, omega-dihydroxy polysiloxane, its viscosity is 5000cp～50000cp, and between different viscosity, need rational Match to use, its ratio is 5000cp～20000cp: 20000cp～50000cp=1: (0.1～20), to increase its polymerization degree, put forward intensity and the hardness of seal gum.
Described filler is selected from one or several in aerosil, precipitated silica, surface modification silicon-dioxide, surface modified nano calcium carbonate.
Preferably, described coupling agent is the organoalkoxysilane that active function groups (sulfydryl, epoxy group(ing), acyloxy, amino etc.) replaces, specifically can be aminopropyl trimethoxysilane, mercapto propyl group three second/methoxy silane, γ-(2.3 epoxy the third oxygen) propyl trimethoxy silicane, at least one in γ-(methacryloxypropyl) propyl trimethoxy silicane etc.
Preferably, water glass curing agent of the present invention, for accelerating solidifying of water glass, comprises organic ester, ferrosilicon powder, beta-dicalcium silicate, Sodium Silicofluoride etc.
Further, organic ester, the example that can enumerate, comprises methyl-formiate, methyl acetate, ethyl acetate, ethyl formate, ten DAADBSA methyl esters, ten DAADBSA ethyl esters, ten DAADBSA isobutyl esters.
Preferably, as the solidifying agent of silicate bond thing, can be above-mentioned solidifying agent separately as the solidifying agent of water glass, can be also that the mixture of above-mentioned solidifying agent is as the solidifying agent of water glass.
Preferably, the solidifying agent agent usage quantity of silicate bond thing is the 0.5%-40% of silicate bond amount.Be more preferably 5%-30%.More preferably, 10%-20%.
Above-mentioned ferrosilicon powder, beta-dicalcium silicate, Sodium Silicofluoride also can be used as fireproofing agent or the fire retardant of two component fire prevention silicone sealants.
in B component:
The water glass cohesive action that act as the two component silicone sealants of reinforcement in the present invention, also can play the effect of fire protection flame retarding.
Water glass refers to water glass or potassium silicate aqueous solution, but the neusilin aqueous solution, the lithium silicate aqueous solution, the lithium magnesium silicate aqueous solution, and the Magnesium Silicate q-agent aqueous solution, also can play the effect identical with water glass in the present invention.Certainly, above-mentioned sodium silicate aqueous solution, potassium silicate aqueous solution, the neusilin aqueous solution, the lithium silicate aqueous solution, the lithium magnesium silicate aqueous solution, the mixture of the Magnesium Silicate q-agent aqueous solution also can play the effect in the present invention.
Linking agent:
In general, described linking agent is general formula R '-Si (R ")
3compound,
Wherein R ' is alkyl, C1-C10 alkyl for example, as methyl, ethyl, propyl group, butyl, amyl group, 2-ethylhexyl, octyl group, decyl, thiazolinyl, C2-C6 alkenyl for example, as vinyl, allyl group, hexenyl, or cycloalkyl, for example C3-C8 cycloalkyl, as cyclopentyl, cyclohexyl and suberyl, aryl, C6-C8 aromatic hydrocarbyl for example, as phenyl, tolyl and xylyl; R " be alkoxyl group, C1-C6 alkoxyl group for example, as methoxyl group, oxyethyl group, propoxy-, butoxy, pentyloxy, aminooxy, C1-C4 acyloxy, C2-C5 alkene oxygen base group or C1-C5 alkyl ketone oximido.
The present invention's " alkyl " used refers to the complete saturated alkyl of straight or branched, can be C1-C10 alkyl, preferably C1-C8 alkyl, more preferably C1-C7 alkyl, particularly preferably C1-C6 alkyl, most preferably C1-C6 alkyl.Example includes but not limited to methyl, ethyl, propyl group, normal-butyl, isobutyl-etc.
The present invention's " thiazolinyl " used refers to the alkyl that comprises one or more pairs of keys in side chain or straight chain hydrocarbon chain, can be C2-C6 thiazolinyl, preferably C2-C5 thiazolinyl, more preferably C2-C4 thiazolinyl, particularly preferably C2-C3 thiazolinyl, most preferably vinyl.Example includes but not limited to vinyl, allyl group, 1-propenyl, 2-propenyl, hexenyl etc.
The present invention's " cycloalkyl " used refers to saturated hydrocarbon ring completely, can be the cycloalkyl of C3-C8, preferably the cycloalkyl of C4-C7.The example of group of naphthene base includes but not limited to cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl etc.
The present invention's " alkoxyl group " used refers to the alkoxyl group of side chain or straight chain.Can be C1-C6 alkoxyl group, preferred C1-C4 alkoxyl group, example includes but not limited to methoxyl group, oxyethyl group, propoxy-, butoxy, isobutoxy, pentyloxy etc.
Described linking agent, linking agent is many alkoxyl silicones alkanes preferably, as in methyltrimethoxy silane, dimethyldimethoxysil,ne, Union carbide A-162, poly-Union carbide A-162, ethyl trimethoxy silane, diethyl diethoxy silane, vinyltrimethoxy silane, vinyltriethoxysilane, tetraethoxy or positive silicic acid propyl ester any one or multiple.
Described chainextender is selected from least one in ethylene methacrylic two (N-methylacetamide base) silane or dimethyl two (N-methylacetamide base) silane.
Preferably, described catalyzer is organo-tin compound.Further preferably, described organo-tin compound is to be selected from dibutyl tin laurate, two lauric acid diamyl tin, two lauric acid dihexyl tin, two dioctyltin laurate, dibutyltin diacetate, two acetic acid diamyl tin, two acetic acid dihexyl tin, two acetic acid dioctyl tins, dimethoxy dibutyl tin, dimethoxy diamyl tin, dimethoxy dihexyl tin, dimethoxy dioctyl tin, diethoxy dibutyl tin, diethoxy diamyl tin, diethoxy dihexyl tin, diethoxy dioctyl tin, dipropoxy dibutyl tin, dipropoxy diamyl tin, dipropoxy dihexyl tin, dipropoxy dioctyl tin, dibutoxy dibutyl tin, dibutoxy diamyl tin, dibutoxy dihexyl tin, dibutoxy dioctyl tin, dibutyl tin diacetyl acetonate, any one in stannous octoate, two kinds or more of.
Organo-tin compound is more preferably any one in dibutyl tin laurate, dibutyltin diacetate, two dioctyltin laurate.
In addition, the two component silicone sealants of fire prevention of the present invention, also comprise inorganic combustion inhibitor.Described inorganic combustion inhibitor is in A component.
As for inorganic fire-retarded compound of the present invention, this inorganic fire-retarded compound at high temperature has good heat absorption capacity, simultaneously non-combustible, play fp effect, particularly, for hydroxide form inorganic combustion inhibitor, oxide type inorganic combustion inhibitor, borate type fire retardant, stannate type fire retardant, antimony type fire retardant, they can be used alone or with two or more kinds of array configuration use.
Further, as hydroxide form fire retardant, the example that can enumerate comprises aluminium hydroxide, magnesium hydroxide, magnesium basic carbonate, ventilation breather, hydrotalcite type complex metal hydroxide, the product that hydrotalcite type complex metal hydroxide is dry.
Further, as oxide type fire retardant, the example that can enumerate, comprises product, rare earth oxide that aluminum oxide, magnesium oxide, cupric oxide, Red copper oxide, ferric oxide, zinc oxide, stannic oxide, hydrotalcite type complex metal hydroxide are calcined.
Further, fire-retardant as borate type, the example that can enumerate comprises zinc borate, barium borate, lime borate, zinc metaborate, barium metaborate.Zinc borate zinc ANTIMONY TRIOXIDE SB 203 99.8 PCT
Further, as stannic acid type fire retardant, the example that can enumerate comprises zinc, barium stannate, alkali formula zinc, alkali formula barium stannate.
Further, as antimony type fire retardant, the example that can enumerate, comprising: ANTIMONY TRIOXIDE SB 203 99.8 PCT, antimony pentaoxide, sodium antimonate, potassium antimonate.
As fire-retardant mineral compound, preferably, hydroxide form fire retardant of the present invention, or oxide type fire retardant arranged in pairs or groups a small amount of by hydroxide form fire retardant.
Preferably, inorganic combustion inhibitor of the present invention is selected the mixture of magnesium hydroxide or aluminium hydroxide or aluminium hydroxide and cerium oxide.
Preferably, the consumption of inorganic combustion inhibitor of the present invention is 20-100 weight part (take α, alpha, omega-dihydroxy polysiloxane is benchmark for 100 weight parts)
The preparation method of the two component silicone sealants of fire prevention of the present invention is identical with the preparation method of common double component silicone seal gum.Be not repeated herein.
Beneficial effect of the present invention:
1. the present invention, by adding water glass, strengthens the viscosifying power of silicone sealant, has guaranteed the fire retardant performance of silicone sealant simultaneously.
2. the present invention, by certain proportioning, has realized workability, the shelf characteric identical with common double component silicone sealant.
Embodiment
embodiment 1-5
Silicone sealant of the present invention, embodiment 1-5 is composed as follows:
A component and B component are prepared respectively to A, B component that A component is uniformly dispersed after dehydration, B component obtains fire protection flame retarding silicone sealant after being uniformly dispersed.
embodiment 6-10
Embodiment 6-10 is corresponding with embodiment 1-5 respectively, and difference is only, in embodiment 6-10, contains inorganic combustion inhibitor, the inorganic combustion inhibitor of embodiment 6-10 in A component, wherein,
Embodiment 6 magnesium hydroxide 20 weight parts
Embodiment 7 aluminum oxide 50 weight parts
Embodiment 8 magnesium hydroxide 20 weight part cerium oxide 5 weight parts
Embodiment 9 zinc borate 100 weight parts
Embodiment 10 zinc 50 weight part ANTIMONY TRIOXIDE SB 203 99.8 PCT 10 weight parts
According to the preparation method of 1-5, prepare fire prevention silicone sealant.
The fire prevention silicone sealant that embodiment 1-10 is obtained, its performance is as following table:
Wherein:
Tensile strength and elongation at break: by standard GB/T/T528-1998, test, the offset plate thickness of preparation is 2.0mm ± 0.2mm, and length is not less than 25mm ± 0.5mm, cut every group, sample and be not less than 5.
Oxygen index method is measured flame retardant properties: by standard GB/T/T10707-1989, measure.Prepare the long 80～150mm of offset plate specimen size, wide 6.5 ± 0.5mm, thick 3 ± 0.25mm.Every kind of offset plate sample is prepared 20. and every group of model test data averaged.
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Tensile strength/MPa | 7.13 | 7.11 | 7.56 | 7.76 | 7.47 |
| Elongation at break/% | 112 | 135 | 149 | 123 | 137 |
| Flame retardant properties/% | 37.6 | 33.2 | 36.7 | 38.5 | 35.9 |
| Performance | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 |
| Tensile strength/MPa | 7.02 | 6.88 | 6.93 | 7.33 | 7.25 |
| Elongation at break/% | 108 | 128 | 137 | 117 | 128 |
| Flame retardant properties/% | 39.7 | 35.4 | 38.7 | 40.2 | 41.5 |
By above-mentioned data, can draw, silicone sealant of the present invention, when guaranteeing flame retardant properties, also has good mechanical property.
Claims (8)
1. two component fire prevention silicone sealants, is characterized in that being comprised of A component and B component, and described A component is comprised of the component of following weight parts:
α, alpha, omega-dihydroxy polysiloxane 100 weight parts;
Polydimethylsiloxane 15-80 weight part;
Filler 50-150 weight part;
Silane coupling agent 0.2-2 weight part;
Water glass curing agent 0.1-10 weight part;
Described B component is comprised of the component of following weight parts:
Water glass 5-50 weight part;
Linking agent 0.5-10 weight part;
Silane coupling agent 0.2-2 weight part;
Chainextender 0.05-1 weight part;
Catalyzer 0.1-5 weight part.
2. a kind of pair of component fire prevention silicone sealant according to claim 1, it is characterized in that, described α, alpha, omega-dihydroxy polysiloxane, its viscosity is 5000cp～50000cp, and between different viscosity, need rational Match to use, its ratio is 5000cp～20000cp: 20000cp～50000cp=1: (0.1～20).
3. a kind of pair of component fire prevention silicone sealant according to claim 1, is characterized in that, described filler is selected from one or several in aerosil, precipitated silica, surface modification silicon-dioxide, surface modified nano calcium carbonate.
4. a kind of pair of component fire prevention silicone sealant according to claim 1, it is characterized in that, described coupling agent is selected from aminopropyl trimethoxysilane, mercapto propyl group three second/methoxy silane, γ-(2.3 epoxy the third oxygen) propyl trimethoxy silicane, at least one in γ-(methacryloxypropyl) propyl trimethoxy silicane.
5. a kind of pair of component fire prevention silicone sealant according to claim 1, it is characterized in that, described water glass curing agent is selected from one or several in ferrosilicon powder, beta-dicalcium silicate, Sodium Silicofluoride, methyl-formiate, methyl acetate, ethyl acetate, ethyl formate, ten DAADBSA methyl esters, ten DAADBSA ethyl esters, ten DAADBSA isobutyl esters.
6. a kind of pair of component fire prevention silicone sealant according to claim 1, it is characterized in that, described linking agent be selected from methyltrimethoxy silane, dimethyldimethoxysil,ne, Union carbide A-162, poly-Union carbide A-162, ethyl trimethoxy silane, diethyl diethoxy silane, vinyltrimethoxy silane, vinyltriethoxysilane, tetraethoxy or positive silicic acid propyl ester any one or multiple.
7. a kind of pair of component fire prevention silicone sealant according to claim 1, is characterized in that, described chainextender is selected from least one in ethylene methacrylic two (N-methylacetamide base) silane or dimethyl two (N-methylacetamide base) silane.
8. a kind of pair of component fire prevention silicone sealant according to claim 1, it is characterized in that, described catalyzer is selected from dibutyl tin laurate, two lauric acid diamyl tin, two lauric acid dihexyl tin, two dioctyltin laurate, dibutyltin diacetate, two acetic acid diamyl tin, two acetic acid dihexyl tin, two acetic acid dioctyl tins, dimethoxy dibutyl tin, dimethoxy diamyl tin, dimethoxy dihexyl tin, dimethoxy dioctyl tin, diethoxy dibutyl tin, diethoxy diamyl tin, diethoxy dihexyl tin, diethoxy dioctyl tin, dipropoxy dibutyl tin, dipropoxy diamyl tin, dipropoxy dihexyl tin, dipropoxy dioctyl tin, dibutoxy dibutyl tin, dibutoxy diamyl tin, dibutoxy dihexyl tin, dibutoxy dioctyl tin, dibutyl tin diacetyl acetonate, any one in stannous octoate, two kinds or more of.
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| CN201310115381.3A CN104099060B (en) | 2013-04-03 | 2013-04-03 | Two-composition fireproof silicone sealant |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315008A (en) * | 2015-10-16 | 2016-02-10 | 江苏名和集团有限公司 | Concrete surface reinforcing sealant and preparation method thereof |
| CN108410407A (en) * | 2018-04-19 | 2018-08-17 | 滁州君越高分子新材料有限公司 | A kind of preparation method of halogen-free flame-retardant adhesive |
| CN110003844A (en) * | 2019-04-24 | 2019-07-12 | 陈果 | A kind of preparation method of ceramic fire prevention silicone sealant |
| CN110257002A (en) * | 2019-05-23 | 2019-09-20 | 宁波聚力新材料科技有限公司 | A kind of Projecting Lamp two-component silicone sealant |
| WO2021004557A1 (en) * | 2019-07-05 | 2021-01-14 | First Point a.s. | Compound for surface protection |
| CN112331391A (en) * | 2020-10-28 | 2021-02-05 | 江苏亿致通信科技有限公司 | High-compression-resistance, noise-resistant, flame-retardant and high-temperature-resistant cable |
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| CN101851083A (en) * | 2010-04-09 | 2010-10-06 | 杨柯 | Artificial building stones and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315008A (en) * | 2015-10-16 | 2016-02-10 | 江苏名和集团有限公司 | Concrete surface reinforcing sealant and preparation method thereof |
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| WO2021004557A1 (en) * | 2019-07-05 | 2021-01-14 | First Point a.s. | Compound for surface protection |
| CN114051546A (en) * | 2019-07-05 | 2022-02-15 | 第一点有限公司 | Composite for surface protection |
| CN112331391A (en) * | 2020-10-28 | 2021-02-05 | 江苏亿致通信科技有限公司 | High-compression-resistance, noise-resistant, flame-retardant and high-temperature-resistant cable |
| CN112331391B (en) * | 2020-10-28 | 2022-04-22 | 江苏亿致通信科技有限公司 | High-compression-resistance, noise-resistant, flame-retardant and high-temperature-resistant cable |
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Effective date of registration: 20180904 Address after: 224100 Yancheng City 1 new building, Jiangsu Hua Hua Industrial Park, Dafeng District, Yancheng City, Jiangsu Patentee after: Jiangsu Hua Si new Mstar Technology Ltd Address before: 201706 No. 1358, Zhao heavy road, Qingpu District, Shanghai Patentee before: SHANGHAI HUAGUI SPECIAL CHEMICALS CO., LTD. |
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Denomination of invention: Two-composition fireproof silicone sealant Effective date of registration: 20200703 Granted publication date: 20150708 Pledgee: Yancheng SME Financing Guarantee Co.,Ltd. Pledgor: Jiangsu Hua Si new Mstar Technology Ltd. Registration number: Y2020980003791 |
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