CN108047970A - A kind of good silicone sealant of weatherability and preparation method thereof - Google Patents
A kind of good silicone sealant of weatherability and preparation method thereof Download PDFInfo
- Publication number
- CN108047970A CN108047970A CN201711320872.6A CN201711320872A CN108047970A CN 108047970 A CN108047970 A CN 108047970A CN 201711320872 A CN201711320872 A CN 201711320872A CN 108047970 A CN108047970 A CN 108047970A
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- silicone sealant
- reaction kettle
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
This case is related to good silicone sealant of a kind of weatherability and preparation method thereof, raw material is matched according to specified weight part and formed by α, the poly- dimethoxysiloxane of ω dihydroxy, trimethyl dimethyl silicone polymer, paraffin oil, organotin, Polycarbosilane, dimethyl divinyl silane, inorganic filler, three ketoximinosilanes of vinyl and pigment；Temperature and stir speed (S.S.) when order of addition to preparation process items raw material and reaction by test of many times and determine optimal preparation method；Single-component room temperature vulcanized silicone sealant good weatherability prepared by the present invention, it is influenced by external conditions such as sunlight, temperature change, wind and weathers weak, it is less prone to the aging phenomena such as cracking, flavescence or adhesion strength decline, the ability of especially resisting ultraviolet irradiation aging is strong, has excellent persistence.
Description
Technical field
The invention belongs to seal sizing material fields, and in particular to a kind of good silicone sealant of weatherability and its preparation side
Method.
Background technology
Room temperature sealing silicone sulfide glue (RTV) is a kind of new elastomer silicone to come out in the sixties in last century,
The characteristics of this rubber is most prominent is without heating, can crosslink curings at ambient temperature, and use extremely facilitates, one
It is born and just is widely used in building as adhesive, sealant, protective coating, embedding and pattern-making material etc., be fitted up, machinery system
It makes, the fields such as chemical industry and electronics.RTV is divided into one-component and two-component, wherein one component room temperature sulphur according to the packaged form of product
SiClx ketone seal gum generates the change of physical property by moisture, that is, water in ingress of air and crosslinking curing；Two-component room temperature sulphur
SiClx ketone seal gum is divided into two groups of A, B, and any group of individualism cannot all form curing, but two groups of rubber cements produce once mixing
It is raw to cure, the condensed room temperature vulcanized silicone sealant of two-component and dual composition addition type room temperature sulphur can be divided into again according to curing mechanism
SiClx ketone seal gum.
The basic material of single-component room temperature vulcanized silicone sealant includes：Polymer, plasticizer, crosslinking agent, filler, catalysis
Basic material is usually uniformly mixed by agent, tackifier, pigment and additive etc. in the dry state, is dispensed and is sealed
, it is uniform and sticky paste in dry conditions, when use squeezes out sizing material, and the moisture in ingress of air occurs
Condensation reaction, crosslinking become elastomer；Because it is easy to use, performance is stable, cheap, single-component room temperature vulcanized silicone seal
Glue is suitable for outdoor and site operation, indoor decoration and the repairing of various occasions more；Due to being chiefly used in open air, one component room temperature sulphur
Changing silicone sealant needs the test through climate, comprehensive as caused by illumination, cold and hot, wind and rain, bacterium etc. to destroy, it is resistant to
Ability, that is, weatherability has higher requirement, and the sealant only with good weatherability properties could keep excellent in longer time
It seals or coheres effect.
The content of the invention
For the shortcoming of silicone sealant in the prior art, it is an object of the invention to provide a kind of weatherability is good
Silicone sealant and preparation method thereof.
The present invention provides a kind of good silicone sealants of weatherability, are made of the raw material of following parts by weight：
Preferably, the inorganic filler is selected from aerosil, glass fibre, gas-phase silica, nano-calcium carbonate
In one or more.
Preferably, the organotin is any one of dibutyl tin laurate, tin dilaurate dioctyl tin.
Preferably, the one kind of the pigment in titanium dioxide, carbon black, aluminium silver powder, rust red.
Preferably, the silicone sealant is made of the raw material that following weight matches：α, the poly- dimethoxy of alpha, omega-dihydroxy
85 parts of siloxanes, 10 parts of paraffin oil, 8 parts of trimethyl dimethyl silicone polymer, 1 part of dibutyl tin laurate, Polycarbosilane 12
Part, 0.8 part of dimethyl divinyl silane, 15 parts of aerosil, 3 parts of three ketoximinosilanes of vinyl, 8 parts of titanium dioxide.
The preparation method of silicone sealant according to the present invention, comprises the following steps：
(1) by α, the poly- dimethoxysiloxane of alpha, omega-dihydroxy, trimethyl dimethyl silicone polymer and paraffin oil add in reaction
In kettle, be warming up to 108-112 DEG C be stirred under vacuum 3.5-4 it is small when, base-material is made；
(2) temperature of reaction kettle is maintained 90-95 DEG C, Polycarbosilane and dimethyl divinyl silicon is added in into reaction kettle
Alkane is stirred under vacuum 50-60 minutes；
(3) reaction kettle is cooled to 40-45 DEG C, three ketoximinosilanes of inorganic filler and vinyl is added in into reaction kettle,
It is stirred under vacuum 10-15 minutes；
(4) organotin and pigment are added in into reaction kettle, be sufficiently stirred under vacuum condition 1 it is small when, obtain silicone sealant
Product.
Preferably, step (1) to the rotating speed stirred described in step (4) is 120-150rpm.
Elaboration to the present invention and its advantage：Single-component room temperature vulcanized silicone sealant prepared by the present invention is weather-proof
Property it is good, influenced by external conditions such as sunlight, temperature change, wind and weathers weak, be less prone to cracking, flavescence or bond strong
The aging phenomena such as degree decline, the ability of especially resisting ultraviolet irradiation aging is strong, has excellent persistence；First, raw material
In α, the poly- dimethoxysiloxane of alpha, omega-dihydroxy, trimethyl dimethyl silicone polymer and paraffin oil mediate after as routine
Silicone sealant base ingredient；Polycarbosilane and dimethyl divinyl the silane cross-linking reaction at a high temperature of 90-95 DEG C generate
Be carbonized silicon original material, can keep sealing glue elasticity and cohesive force in the case of be formed on its surface protective layer, effectively resist because
The damage that external environment change, soda acid influence, bacterial corrosion etc. are brought to fluid sealant, especially can effectively resist ultraviolet illumination
Damage greatly improves the weatherability of fluid sealant product；Three ketoximinosilanes of vinyl can both be used as crosslinking agent, enhancing sealing
The inner structural strength of glue, and there is certain antibacterial action in system, it can prevent erosion of the bacterium to bonding system
Mouldization.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
Embodiment 1
Raw material forms (parts by weight)：α, 85 parts of the poly- dimethoxysiloxane of alpha, omega-dihydroxy, 10 parts of paraffin oil, trimethyl gather
8 parts of dimethyl siloxane, 1 part of dibutyl tin laurate, 12 parts of Polycarbosilane, 0.8 part of dimethyl divinyl silane, gas phase
5 parts of silica 1,3 parts of three ketoximinosilanes of vinyl, 8 parts of titanium dioxide.
Preparation method：
(1) by α, the poly- dimethoxysiloxane of alpha, omega-dihydroxy, trimethyl dimethyl silicone polymer and paraffin oil add in reaction
In kettle, be warming up to 108-112 DEG C be stirred under vacuum 3.5-4 it is small when, base-material is made；
(2) temperature of reaction kettle is maintained 90-95 DEG C, Polycarbosilane and dimethyl divinyl silicon is added in into reaction kettle
Alkane is stirred under vacuum 50-60 minutes；
(3) reaction kettle is cooled to 40-45 DEG C, aerosil and vinyl triketone oximido silicon is added in into reaction kettle
Alkane is stirred under vacuum 10-15 minutes；
(4) dibutyl tin laurate and titanium dioxide are added in into reaction kettle, be sufficiently stirred under vacuum condition 1 it is small when, obtain
To silicone sealant product.
Embodiment 2
Raw material forms (parts by weight)：α, 80 parts of the poly- dimethoxysiloxane of alpha, omega-dihydroxy, 8 parts of paraffin oil, trimethyl poly- two
8 parts of methylsiloxane, 0.8 part of dibutyl tin laurate, 10 parts of Polycarbosilane, 1 part of dimethyl divinyl silane, glass fibers
16 parts of dimension, 3 parts of three ketoximinosilanes of vinyl, 8 parts of carbon black.
Each raw material composition is had adjusted in limited range of the present invention and proportion, preparation method are same as Example 1.
Comparative example 1
Raw material forms (parts by weight)：α, 85 parts of the poly- dimethoxysiloxane of alpha, omega-dihydroxy, 10 parts of paraffin oil, trimethyl gather
8 parts of dimethyl siloxane, 1 part of dibutyl tin laurate, 2 parts of Polycarbosilane, 10 parts of silicon carbide fibre, dimethyl divinyl
0.8 part of silane, 15 parts of aerosil, 3 parts of three ketoximinosilanes of vinyl, 8 parts of titanium dioxide.
The Polycarbosilane content in embodiment 1 is reduced, is directly replaced with silicon carbide fibre, in step in preparation process
(2) silicon carbide fibre is added in, remaining preparation process is same as Example 1.
Comparative example 2
Raw material forms (parts by weight)：α, 85 parts of the poly- dimethoxysiloxane of alpha, omega-dihydroxy, 10 parts of paraffin oil, trimethyl gather
8 parts of dimethyl siloxane, 1 part of dibutyl tin laurate, 12 parts of Polycarbosilane, 0.8 part of vinyltrimethoxysilane, gas phase
5 parts of silica 1,3 parts of three ketoximinosilanes of vinyl, 8 parts of titanium dioxide.
The dimethyl divinyl silane in embodiment 1 is replaced with same amount of vinyltrimethoxysilane,
Remaining preparation process is same as Example 1.
Comparative example 3
Current season the best silicone sealant of sales volume.
For the weatherability of silicone sealant in testing example 1-2 and comparative example 1-3, first according to GB/T528-2009
The tensile strength and elongation at break of fluid sealant product are measured with electronic universal tester, is measured and sealed according to GB/T529-2008
The tearing strength of glue；Then product is placed in burn-in chamber and simulates nature environment progress burnin operation, then test aging respectively
The tensile strength of fluid sealant, elongation at break and tearing strength afterwards；Test result is all recorded in table 1.
According to test result as can be seen that silicone sealant prepared by according to the present invention, i.e. embodiment 1 and embodiment 2,
Preferable performance is shown in items are tested, especially before and after burnin operation, tensile strength, elongation at break and is torn
The numerical value change of resistance to spalling is no more than 5%, has preferable resistance to ag(e)ing and weatherability；Comparative example 1 and comparative example 2 are in raw material
To Polycarbosilane, either the dosage of vinyltrimethoxysilane or composition are changed on composition, although it is before ageing
Properties be not much different with embodiment 1, but its hydraulic performance decline is larger after weathering, and especially tearing strength reduces closely
18%, this illustrates that Polycarbosilane and vinyltrimethoxysilane mutually act synergistically in silicone sealant system, Neng Gouyou
The ageing-resistant performance and weather resistance of raising system are imitated, Neither of the two can be dispensed；Pass through embodiment 1 and the test result of comparative example 3
Compare, it is found that similar production of the silicone sealant in terms of mechanical property and weatherability more on the market prepared by the present invention
Product are significantly improved.
Table 1
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, it is of the invention and unlimited
In specific details.
Claims (7)
1. a kind of good silicone sealant of weatherability, which is characterized in that be made of the raw material of following parts by weight：
2. silicone sealant according to claim 1, which is characterized in that the inorganic filler be selected from aerosil,
One or more in glass fibre, gas-phase silica, nano-calcium carbonate.
3. silicone sealant according to claim 1, which is characterized in that the organotin for dibutyl tin laurate,
Any one of tin dilaurate dioctyl tin.
4. silicone sealant according to claim 1, which is characterized in that the pigment is selected from titanium dioxide, carbon black, aluminium silver
One kind in powder, rust red.
5. according to claim 1 gained silicone sealant, which is characterized in that the raw material matched by following weight forms：α, ω-two
85 parts of the poly- dimethoxysiloxane of hydroxyl, 10 parts of paraffin oil, 8 parts of trimethyl dimethyl silicone polymer, dibutyl tin laurate 1
Part, 12 parts of Polycarbosilane, 0.8 part of dimethyl divinyl silane, 15 parts of aerosil, three ketoximinosilanes 3 of vinyl
Part, 8 parts of titanium dioxide.
6. a kind of preparation method of silicone sealant according to claim 1, which is characterized in that comprise the following steps：
(1) by α, the poly- dimethoxysiloxane of alpha, omega-dihydroxy, trimethyl dimethyl silicone polymer and paraffin oil add in reaction kettle
In, be warming up to 108-112 DEG C be stirred under vacuum 3.5-4 it is small when, base-material is made；
(2) temperature of reaction kettle is maintained 90-95 DEG C, Polycarbosilane and dimethyl divinyl silane is added in into reaction kettle,
It is stirred under vacuum 50-60 minutes；
(3) reaction kettle is cooled to 40-45 DEG C, three ketoximinosilanes of inorganic filler and vinyl, vacuum is added in into reaction kettle
Stirring 10-15 minutes；
(4) organotin and pigment are added in into reaction kettle, be sufficiently stirred under vacuum condition 1 it is small when, obtain silicone sealant product.
7. preparation method according to claim 6, which is characterized in that step (1) to the rotating speed stirred described in step (4)
For 120-150rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711320872.6A CN108047970A (en) | 2017-12-12 | 2017-12-12 | A kind of good silicone sealant of weatherability and preparation method thereof |
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| CN201711320872.6A CN108047970A (en) | 2017-12-12 | 2017-12-12 | A kind of good silicone sealant of weatherability and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111635633A (en) * | 2020-06-12 | 2020-09-08 | 苏州九维电气制造有限公司 | High-stability self-curing insulation protection packaging material and preparation method thereof |
| CN113621336A (en) * | 2021-07-28 | 2021-11-09 | 杭州之江新材料有限公司 | High-temperature curing silane modified polyether sealant and preparation method and use method thereof |
| CN114149767A (en) * | 2021-12-21 | 2022-03-08 | 宝美施化工(上海)有限公司 | Weather-resistant temperature-resistant inorganic silicone adhesive color paste and preparation method and application thereof |
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