CN107325781A - Silicone sealant compositions, organosilicon sealant and preparation method thereof - Google Patents

Silicone sealant compositions, organosilicon sealant and preparation method thereof Download PDF

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Publication number
CN107325781A
CN107325781A CN201610277900.XA CN201610277900A CN107325781A CN 107325781 A CN107325781 A CN 107325781A CN 201610277900 A CN201610277900 A CN 201610277900A CN 107325781 A CN107325781 A CN 107325781A
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fire retardant
weight
parts
sealant
sealant compositions
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林信平
张玲玲
徐斌
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BYD Co Ltd
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BYD Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • C09J183/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/541Silicon-containing compounds containing oxygen
    • C08K5/5425Silicon-containing compounds containing oxygen containing at least one C=C bond
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • C08K2003/387Borates

Abstract

The present invention relates to fluid sealant field.For solution, inorganic fire-retarded class fluid sealant flame retarding efficiency is low in the prior art, difficult processing, the problem of quality guarantee period is short, and the invention discloses a kind of silicone sealant compositions, said composition contains:Base rubber, deicer, stabilizer, tackifier, catalyst and fire retardant;The base rubber is alkoxy end-capped dimethyl silicone polymer;The fire retardant is made up of Firebrake ZB and hydroxide, and the weight ratio of the Firebrake ZB and hydroxide is 1:1‑9;The fire retardant is modified by coupling agent.Present invention also offers the method for preparing organosilicon sealant using above-mentioned composition, and by its obtained organosilicon sealant.There is high flame retardant by using organosilicon sealant made from the composition of the present invention, while having excellent mechanical property and longer storage period concurrently.

Description

Silicone sealant compositions, organosilicon sealant and preparation method thereof
Technical field
The present invention relates to a kind of silicone sealant compositions, organosilicon sealant and preparation method thereof.
Background technology
There is the flame retardant type organosilicon sealant compared with polymorphic type in the market, although existing product has preferable fire resistance and adhesive property, but can not still meet some has use condition compared with high fire-retardance and seal request, such as, the adhering and sealing of high temperature radiating copper base, fixation of heavy-duty motor circuit etc..In this type of application, it is desirable to which used fluid sealant is to have preferable fire resistance and adhesive property, in addition it is also necessary to have higher intensity.Therefore, to sealant formula, the selection of especially base material and fire proofing has high requirement.
In view of Environmental Factors, fire retardant can not be used as using brominated flame-retardant, the fire retardant containing heavy metal and traditional melamine class material in fluid sealant;And more efficient organophosphorous fire retardant cost is very high and poor with the compatibility of silica gel system;And inorganic combustion inhibitor such as magnesium hydroxide, aluminium hydroxide etc., although all there is advantage in the feature of environmental protection and cost, but flame retarding efficiency is low, and generally requiring larger addition just can make fluid sealant reach specific flame retardant effect and intensity.Meanwhile, influenceed between these hydroxide flame retardants and base rubber by hydrogen bond, with stronger interaction, the viscosity of sizing material can be made to increase rapidly in batch mixing, or even recurring structure, so that the production preparation to fluid sealant brings difficulty.
Moreover, the higher organosilicon sealant of inorganic combustion inhibitor loading is during storage, because hydroxide flame retardant therein can be decomposed gradually, produce steam, the small-molecule substances such as crosslinking agent, coupling agent in fluid sealant react, system stability is set to be deteriorated, it may appear that gel, or the situation that extrusion does not solidify.Therefore, the shelf-life of this kind of organosilicon sealant is often shorter.
The content of the invention
For solution, inorganic fire-retarded class fluid sealant flame retarding efficiency is low in the prior art, difficult processing, the problem of quality guarantee period is short, invention, which is provided in a kind of silicone sealant compositions, the silicone sealant compositions, contains base rubber, deicer, stabilizer, tackifier, catalyst and fire retardant;The base rubber is alkoxy end-capped dimethyl silicone polymer;The fire retardant is made up of Firebrake ZB and hydroxide, and the weight ratio of the Firebrake ZB and hydroxide is 1:1-9;The fire retardant is modified by coupling agent.
Inventor in the application has found have cooperative effect when adding hydroxide and Firebrake ZB flame-retardant composition in alkoxy end-capped dimethyl silicone polymer base rubber, can give play to good flame retardant effect by many experiments.Meanwhile, these fire retardant powders are also reinforced filling simultaneously, by coupling agent to powder-modified, the powder filled amount of increase that can be largely, substantially increase fluid sealant fire resistance and mechanical property.
The present invention also provides a kind of preparation method of organosilicon sealant, and this method includes being mixed the composition that above-mentioned composition contains.
Present invention also offers the organosilicon sealant as made from the above method.
The organosilicon sealant obtained by the present invention has preferable fire resistance(Up to V-0 grades of UL94), have excellent mechanical property concurrently, its tensile shear strength is up to 4.0MPa, elongation at break 40%;And any poisonous and hazardous fire retardant is not added with fluid sealant, and only it can discharge a small amount of small molecule alcohol material in the curing process, low VOC, odorlessness is the preferable fire proofing for meeting high-environmental in current industrial production.Moreover, the fluid sealant system stability is improved, and is found through experiments that, product shelf-life below 25 DEG C is 6 months, under the conditions of being somebody's turn to do, and gel caking, situations such as extrusion does not solidify will not occur for fluid sealant.System viscosity is basically unchanged, and can normally be used.
Embodiment
The embodiment to the present invention is described in detail below.It should be appreciated that embodiment described herein is merely to illustrate and explain the present invention, it is not intended to limit the invention.
Technical scheme is related to a kind of organosilicon sealant, and said composition contains:The silicone sealant compositions contain base rubber, deicer, stabilizer, tackifier, catalyst and fire retardant;The base rubber is alkoxy end-capped dimethyl silicone polymer;The fire retardant is made up of Firebrake ZB and hydroxide, and the weight ratio of the Firebrake ZB and hydroxide is 1:1-9;The fire retardant is modified by coupling agent.
Alkoxy end-capped dimethyl silicone polymer is used in the present invention as base rubber, the hydroxy radical content in organic component can largely be reduced, and then hydrogen bond action too strong between organic component and fire retardant powder is reduced, the rising of system viscosity, increases powder filled amount effectively in control mixing process.And selected base rubber is dealcoholized type silica gel, dealcoholized type silica gel be cold curing condensed type silica gel in the most environmentally friendly one kind, it solidifies the alcohol micromolecular environmental sound of release, corrosion-free to bonding base material, and stable components, even if also being released in ablation process without pernicious gas.And the fire retardant selected in the present invention, hydroxide and Firebrake ZB are environment friendly flame retardants, do not contain any composition by environmental protection tests management and control.Therefore, with preferable environmental-protecting performance.
According to present disclosure, the alkoxy end-capped dimethyl silicone polymer of described base rubber material is in the art usually used, is specifically as follows:One or more in the dimethyl silicone polymer that dimethyl silicone polymer, the trimethoxy of dimethoxy end-blocking are blocked.
Hydroxide in the present invention absorbs heat by pyrolytic and improves the thermal capacitance of system, so as to improve fire resistance;And Firebrake ZB is that combustible and oxygen are isolated by thermal decomposition generation coating to improve fire resistance, there is cooperative effect because both there are different fire retardant mechanisms, when being used in conjunction with, good flame retardant effect can have been given play to.Meanwhile, these fire retardant powders are also reinforced filling simultaneously, so to reach that preferable fire resistance and mechanical property need the key issue solved to be all the loading for improving fire retardant powder in fluid sealant.Under preferable case, on the basis of the base rubber of 100 parts by weight, the consumption of fire retardant is 170-200 parts by weight.When the consumption of Firebrake ZB and hydroxide is 1:During 1-9, under both synergies, flame retardant effect and reinforcing effect can reach most preferably simultaneously.
In the present invention, the fire retardant is to carry out being sufficiently mixed modification by coupling agent and fire retardant powder by coupling agent modified mode.This can be largely increase fire retardant powder loading, fire retardant addition is reached more than 60%, while showing excellent mobility and mechanical property.Under preferable case, the weight ratio of the fire retardant and coupling agent is 40-50:1.Under preferable case, the coupling agent is made up of component A and B component;The component A of the coupling agent is a kind of Long carbon chain silane coupler, and the coupling agent can reduce the surface polarity of fire retardant powder, make it more preferable with organic component compatibility;The B component of the coupling agent is:There is highly polar group and non-polar group simultaneously in its molecule, after the coupling agent modified fire retardant powder, the surface wettability of powder can be increased, promote powder to be dispersed in well among organic component, so as to reduce viscosity.In the case of further preferably, by both coupling agents with 1:1-5:1 ratio, which coordinates, can reach optimum efficiency.
In the present invention, the hydroxide is hydroxide conventional in the art, is specifically as follows aluminium hydroxide and/or magnesium hydroxide.
, according to the invention it is preferred in the case of, the component A of the coupling agent is the one or more in hexadecyl trimethoxy silane, stearic acid, Aluminate;The B component of the coupling agent be gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, γ-(2,3 the third oxygen of epoxy)One or more in propyl trimethoxy silicane.
In the present invention, the deicer is the one or more in vinyltrimethoxy silane, anhydrous calcium chloride, calcium oxide;Under preferable case, on the basis of the base rubber of 100 parts by weight, the consumption of the deicer is 1-6 parts by weight.
In the present invention, the stabilizer is MTMS.Under preferable case, on the basis of the base rubber of 100 parts by weight, the consumption of the stabilizer is 3-5 parts by weight.
In the present invention, the organotin catalysts are the one or more in normal-butyl tin dilaurate tin, stannous oxalate, stannous octoate.Under preferable case, on the basis of the base rubber of 100 parts by weight, the content of the organotin catalysts is 0.1-0.5 parts by weight.
In the present invention, the tackifier can effectively improve the adhesive property of fluid sealant, while good co-catalysis effect can also be played, shorten the surface drying hardening time of fluid sealant, be easy to use, improve efficiency of construction.The tackifier are double amino silane tackifier conventional in the art, one or more in specially N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-aminopropyltrimethoxysilane and γ-(2,3- glycidoxy) propyl trimethoxy silicane.Under preferable case, on the basis of the base rubber of 100 parts by weight, the consumption of the tackifier is 1-2 parts by weight.
Under preferable case, also contain thixotropic agent in the silicone sealant compositions of the present invention, by adding thixotropic agent, flow model product of the viscosity between 100Pas-200Pas and the paste thixotropic product substantially without mobility can be obtained, the demand of different execution conditions can be met.The thixotropic agent is thixotropic agent conventional in the art, the specially one or more in white carbon, nano-calcium carbonate.Under preferable case, the thixotropic agent is fume colloidal silica.Under preferable case, on the basis of the base rubber of 100 parts by weight, the content of thixotropic agent is 0-4 parts by weight.
Present invention also offers a kind of preparation method of organosilicon sealant, this method includes being mixed the composition that above-mentioned composition contains.
Although the method for the present invention can include the method for mixing the composition that above-mentioned composition contains according to any form, for example can be using the method for disposably being mixed the composition that above-mentioned composition contains, or the method mixed in a certain order, wherein, for the method disposably mixed, this method includes:Base rubber, deicer, stabilizer, organotin catalysts and fire retardant are mixed.
The condition of the mixing can for example include:First at a temperature of 90-120 DEG C, mixing 30-90 Min, then again at a temperature of 90-120 DEG C, 600-1500 60-180 min are mixed under rpm rotating speed.This method also includes mixed product carrying out vacuum defoamation, and the condition of the vacuum defoamation can for example include:Vacuum Deposition is -0.1 to -0.05MPa, at a temperature of 15-40 DEG C, with 200-900 rpm rotating speed deaeration 15-45min.
Preferably, the preparation method of organosilicon sealant of the invention in a certain order will be mixed the composition that above-mentioned composition contains, i.e. preferably, this method includes:
(1) base rubber, deicer are mixed;
(2) product of gained in step (1) is added into coupling agent, fire retardant to be mixed;
(3) product of gained in step (2) is mixed with organotin catalysts, stabilizer.
, according to the invention it is preferred in the case of, step(1)Mixing condition include:Temperature is 90-120 DEG C(Preferably 100-120 DEG C), the time is 30-90min(Preferably 45-60 min).The mixing can be in stir speed (S.S.) 300-1000rpm(Preferably 500-900rpm)It is lower to carry out.The mixing of the step can reach the purpose of water removal, and the mixed process can be carried out by the conventional various modes in this area, for example, mixed in power mixer.
, according to the invention it is preferred in the case of, it is additionally added thixotropic agent in step (2).
According to the present invention, the mixing condition of step (3) is:Temperature is 15-40 DEG C(Preferably 15-30 DEG C), the time is 15-90min(Preferably 30-60min).The mixing can be in stir speed (S.S.) 300-1000rpm(Preferably 500-900rpm)It is lower to carry out.Under preferable case, add organotin catalysts in step (3) and mixed with before stabilizer, first adding tackifier with the product of step (2).
Deaeration is carried out according to the present invention it is possible to which step (3) is mixed into products therefrom and is fed through in vacuum degasing machine, the condition of deaeration processing includes:Vacuum is -0.1 to -0.05MPa, and mixing speed is 200-900rpm, and temperature is 15-40 DEG C, and the time is 15-45 min.
According to the present invention, in this method, the base rubber, deicer, thixotropic agent, fire retardant, tackifier, organotin catalysts and stabilizer species and consumption it is as described above, will not be repeated here.
Certainly, organosilicon sealant of the invention is not precluded from other additive components, so long as additive component have no effect on the performance of the organosilicon sealant obtained by the present invention.
It for example can be White Mineral Oil as such additive.These additives can add mixing in above-mentioned arbitrary steps, so long as addition do not interfere with the performance of the organosilicon sealant obtained by the present invention.
Present invention also offers the organosilicon sealant as made from the above method.The organosilicon sealant has preferable fire resistance and mechanical property;And product stability is effectively lifted, it can also keep its system viscosity stable after the storage of long period, satisfaction is normally used.
With reference to embodiments, the present invention is further described in detail, but is not limited to this.
In following examples:
Hexadecyl trimethoxy silane is purchased from Chengdu Guibao Technology Co., Ltd, the trade mark 9116;
Gamma-aminopropyl-triethoxy-silane is purchased from Chengdu Guibao Technology Co., Ltd, trade mark KH-550;
Fume colloidal silica is purchased from EVONIK-DEGUSSA companies, trade mark AEROSIL R974;
Double amino silanes are purchased from Chengdu Guibao Technology Co., Ltd, trade mark A-1120.
Other raw materials in embodiment are for example non-to be refered in particular to, and is commercially available prod.
Embodiment 1
By the alkoxy end-capped dimethyl silicone polymers of 1000g, 10g vinyltrimethoxy silanes are added in power mixer, stirring at low speed, and 120 DEG C of high temperature remove water 1h;Then 30g silane couplers, wherein hexadecyl trimethoxy silane are used before adding(9116)And gamma-aminopropyl-triethoxy-silane(KH-550)Ratio is 3:1, the fire retardant that surface is modified(Aluminium hydroxide and Firebrake ZB ratio are 5:1)1800g, 30g fume colloidal silica, vacuum defoamation, stirring at low speed disperse at a high speed 3h, and material temperature maintains 120 DEG C.Heating is closed afterwards, and sizing material is dropped to room temperature and adds the double amino silanes of 10g by stirring at low speed(A-1120), stir 45min;Then add after 2g organotin catalysts, 30g MTMSs stirring at low speed 45min, vacuum defoamation 30min and discharge, be fitted into standby in teflon seal pipe.Obtain sealant specimen A1.
Embodiment 2
(Without thixotropic agent)
Formula:Dimethyl silicone polymer alkoxy end-capped 1000g, 10g vinyltrimethoxy silane deicers;1800g passes through 30g silane couplers(In coupling agent, 9116 and KH-550 ratios are 3:1)The fire retardant that surface is modified(In fire retardant, aluminium hydroxide and Firebrake ZB ratio are 5:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen A2.
Embodiment 3
Formula:Dimethyl silicone polymer alkoxy end-capped 1000g, 10g vinyltrimethoxy silane deicers;2000g passes through 30g silane couplers(Wherein, 9116 and KH-550 ratios are 5:1)The fire retardant that surface is modified(Wherein, aluminium hydroxide and Firebrake ZB ratio are 9:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen A3.
Embodiment 4
By the alkoxy end-capped dimethyl silicone polymers of 1000g, 10g vinyltrimethoxy silane deicers;1700g passes through 30g silane couplers(Wherein, 9116 and KH-550 ratios are 1:1)The fire retardant that surface is modified(Wherein, aluminium hydroxide and Firebrake ZB ratio are 1:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen A4.
Embodiment 5
It is formulated and is:By the alkoxy end-capped dimethyl silicone polymers of 1000g, 10g vinyltrimethoxy silane deicers;1800g passes through the fire retardant that the surface of 30g silane couplers 9116 is modified(Wherein, aluminium hydroxide and Firebrake ZB ratio are 5:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen A5.
Comparative example 1
(Use single fire retardant)
It is formulated and is:Dimethyl silicone polymer alkoxy end-capped 1000g;10g vinyltrimethoxy silane deicers;1800g passes through 30g silane couplers(Wherein, 9116 and KH-550 ratios are 3:1)The aluminium hydroxide that surface is modified;The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen D1.
Comparative example 2
(Fire-retardant powder is non-modified)
By the alkoxy end-capped dimethyl silicone polymers of 1000g;10g vinyltrimethoxy silane deicers;1800g does not carry out the fire retardant of surface modification(Wherein, aluminium hydroxide and Firebrake ZB ratio are 5:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts;30g MTMSs.Specific preparation technology be the same as Example 1.Obtain sealant specimen D2.
Comparative example 3
It is formulated and is:Dimethyl silicone polymer alkoxy end-capped 1000g;1800g passes through the aluminium hydroxide that 30g silane resin acceptor kh-550s surface is modified;10g vinyltrimethoxy silane deicers;10g silane coupler class tackifier;2g organotitaniums(Titanium propanolate).Obtain sealant specimen D3.
Comparative example 4
(The stable promotion property of MTMS)
It is formulated and is:Dimethyl silicone polymer alkoxy end-capped 1000g;10g vinyl trimethoxy silicon deicers;1800g passes through 30g silane couplers(Wherein, 9116 and KH-550 ratios 3:1)The fire retardant that surface is modified(Wherein, aluminium hydroxide and Firebrake ZB ratio are 5:1);The double amino silane A-1120 tackifier of 10g;2g organotin catalysts.Specific preparation technology embodiment 1.Obtain sealant specimen D4.
Comparative example 5
It is formulated and is:Alkoxy end-capped 107 glue;1800g passes through the aluminium hydroxide that 30g silane resin acceptor kh-550s surface is modified;10g vinyltrimethoxy silane deicers;10g silane coupler class tackifier;2g organotitaniums(Titanium propanolate).Obtain sealant specimen D5.
Performance test:
Above-mentioned experiment is obtained into the D1-D5 in sealant specimen A1-A5 and comparative example to be extruded into polytetrafluoroethylene (PTFE) groove(25±5)℃、(55±5)Solidify 7 days under the conditions of %RH, be then cut into dumbbell shaped sample and carry out performance test.
1st, fire resistance:According to《UL94》Standard is carried out;Wherein, fire resistance is followed successively by V-0, V-1, V-2 from high to low.
2nd, tensile strength and elongation at break:According to《GB/T528-1998》In method carry out;
3rd, shear strength test:According to《GB/T7124》The method of middle offer carries out shear strength test;
4th, surface drying time is determined:(25±5)℃、(55±5)Under the conditions of %RH, appropriate fluid sealant is coated on clean polyfluortetraethylene plate, thickness about 2mm touches glue surface every 1 min with finger, be surface drying time to the tack-free time;
5th, curing rate is tested:300 mm are about with one, and depth is 0-10 mm gradually deep polytetrafluoroethylene (PTFE) skewed slots.Appropriate fluid sealant is extruded in down fold, with doctor blade, does not make have bubble in glue-line,(25±2)℃、(55±5)Glued membrane is uncovered from thinnest part after 24 h are placed under the conditions of %RH, until at uncured adhesion, surveying the depth of groove at this, being represented with mm/24h.
6th, storage performance is tested:The seal pipe that will be equipped with flame retardant sealant is put into preservation in 25 DEG C of dark environment dried, periodically(General 1 month)Sampling, the apparent condition of extrusion observation fluid sealant, and its mechanical property is tested(Repeat above-mentioned test experience), apparent condition and performance change little crash time and be its normal shelf phase.
7th, degradation:The seal pipe that will be equipped with flame retardant sealant is put into preservation in 70 DEG C of baking ovens, is sampled after 3 days, the apparent condition of extrusion observation fluid sealant, and its mechanical property is tested.
The performance test results see the table below 1 ~ table 2.
Table 1 --- embodiment performance test data
Table 2 --- comparative example performance test data
It can be seen that by above-mentioned test:
1. substantially got well collectively as the flame retardant effect that the single use aluminium hydroxide of fire retardant ratio reaches using aluminium hydroxide and Firebrake ZB a lot;
2. system viscosity can be largely reduced using silane coupler modified fire retardant powder, increases powder filled amount;
3. double amino silane tackifier can strengthen the adhesive property of fluid sealant well, and can substantially accelerate the surface drying hardening time of fluid sealant, be easy to construction;
4. the fluid sealant product fire resistance and mechanical property that prior art is obtained will not be all better than products obtained therefrom of the present invention, and surface drying is excessively slow, and surface tack occurs in storage process, it is impossible to situations such as solidifying, and product stability can be bad.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.For those of ordinary skill in the field, it can also make other changes in different forms on the basis of the above description.Among there is no necessity and possibility to exhaust all the enbodiments, and the obvious changes or variations thus extended out is still in the invention scope of the claims.

Claims (15)

1. a kind of silicone sealant compositions, it is characterised in that the silicone sealant compositions contain base rubber, deicer, stabilizer, tackifier, catalyst and fire retardant;The base rubber is alkoxy end-capped dimethyl silicone polymer;The fire retardant is made up of Firebrake ZB and hydroxide, and the weight ratio of the Firebrake ZB and hydroxide is 1:1-9;The fire retardant is modified by coupling agent.
2. silicone sealant compositions according to claim 1, it is characterized in that, on the basis of the base rubber of 100 parts by weight, the consumption of the deicer is 1-6 parts by weight, the consumption of stabilizer is 3-5 parts by weight, the consumption of tackifier is 1-2 parts by weight, and the consumption of organotin catalysts is 0.1-0.5 parts by weight, and the consumption of fire retardant is 170-200 parts by weight.
3. silicone sealant compositions according to claim 1, it is characterised in that the alkoxy end-capped organosiloxane is the one or more in the dimethyl silicone polymer that dimethyl silicone polymer, the trimethoxy that dimethoxy is blocked are blocked.
4. silicone sealant compositions according to claim 1, it is characterised in that hydroxide is aluminium hydroxide and/or magnesium hydroxide in the fire retardant.
5. silicone sealant compositions according to claim 1, it is characterised in that the weight ratio of the fire retardant and coupling agent is 40-50:1.
6. silicone sealant compositions according to claim 1, it is characterised in that the coupling agent is made up of component A and B component;The component A of the coupling agent is the one or more in hexadecyl trimethoxy silane, stearic acid, Aluminate;The B component of the coupling agent be gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, γ-(2,3 the third oxygen of epoxy)One or more in propyl trimethoxy silicane.
7. silicone sealant compositions according to claim 6, it is characterised in that the component A and B component weight ratio of the coupling agent are 1:1-5:1.
8. silicone sealant compositions according to claim 1, it is characterised in that the deicer is the one or more in vinyltrimethoxy silane, anhydrous calcium chloride, calcium oxide;The stabilizer is MTMS;The catalyst is organotin catalysts, and the organotin catalysts are the one or more in normal-butyl tin dilaurate tin, stannous oxalate, stannous octoate.
9. silicone sealant compositions according to claim 1, it is characterized in that, the tackifier are the one or more in N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-aminopropyltrimethoxysilane and γ-(2,3- glycidoxy) propyl trimethoxy silicane;On the basis of the base rubber of 100 parts by weight, the consumption of the tackifier is 1-2 parts by weight.
10. silicone sealant compositions according to claim 1, it is characterised in that contain thixotropic agent in the silicone sealant compositions, the thixotropic agent is the one or more in white carbon, nano-calcium carbonate;On the basis of the base rubber of 100 parts by weight, the consumption of the thixotropic agent is 0-6 parts by weight.
11. a kind of preparation method of organosilicon sealant, it is characterised in that including the composition that the composition described in claim 1-7 any one contains is mixed.
12. organosilicon sealant preparation method according to claim 11, it is characterised in that this method includes:
(1) base rubber, deicer are mixed;
(2) product of gained in step (1) is mixed with coupling agent, thixotropic agent, fire retardant;
(3) product of gained in step (2) is mixed with organotin catalysts, stabilizer.
13. organosilicon sealant preparation method according to claim 12, it is characterised in that the mixing condition in step (1) includes:Temperature is 90-120 DEG C, and the time is 30-90min.
14. organosilicon sealant preparation method according to claim 12, it is characterised in that add organotin catalysts in step (3) and mixed with before stabilizer, first adding tackifier with the product of step (2);The mixing condition includes:Temperature is 15-40 DEG C, and the time is 30-90min.
15. organosilicon sealant made from the method according to any one in claim 11-14.
CN201610277900.XA 2016-04-29 2016-04-29 Silicone sealant compositions, organosilicon sealant and preparation method thereof Pending CN107325781A (en)

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Application publication date: 20171107