CN108559443A - A kind of low modR vulcanization neutral silicone weather proofing sealant and its preparation method and application - Google Patents
A kind of low modR vulcanization neutral silicone weather proofing sealant and its preparation method and application Download PDFInfo
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- CN108559443A CN108559443A CN201810511461.3A CN201810511461A CN108559443A CN 108559443 A CN108559443 A CN 108559443A CN 201810511461 A CN201810511461 A CN 201810511461A CN 108559443 A CN108559443 A CN 108559443A
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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
- 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
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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
- 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
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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
- C09J183/00—Adhesives 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
- C09J183/04—Polysiloxanes
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a kind of low modRs to vulcanize neutral silicone weather proofing sealant, is grouped as by the group calculated by weight as follows:160 ~ 240 parts of base polymer;30 ~ 80 parts of precipitated calcium carbonate;100 ~ 160 parts of powdered whiting;3 ~ 6 parts of graphene oxide;12 ~ 30 parts of dimethicone;8 ~ 15 parts of chain extender;13 ~ 19 parts of crosslinking agent;2.5 ~ 5 parts of coupling agent;0.2 ~ 0.4 part of catalyst;The base polymer is that both ends are hydroxy-end capped dimethyl silicone polymer, and the viscosity at a temperature of 25 DEG C of the base polymer is 60000 ~ 75000mPas.Silicone sealant provided by the invention has low stretch modulus, high resiliency and high elastic recovery rate, and excellent weatherability and good adhesive property, after the processing such as cold drawing-hot pressing, immersion, be not in bonding interface destruction and cohesional failure, it may advantageously facilitate the sealing of the concrete extension joints of facilities such as high displacement joint filling and road, bridge, airfield runway of the silicone sealant in high-rise building.
Description
Technical field
The present invention relates to high molecule sealing materials technical fields, vulcanize more particularly, to a kind of low modR neutral
Silicone weatherproof sealant and its preparation method and application.
Background technology
Modulus refers to material the ratio between stress and strain under stress.Modulus after silicone sealant complete cure can divide
It is three kinds:High-modulus, middle modulus and low modulus.The displacement capacity of low modulus silicone sealant can reach+100/-50, have
The advantages that permanent deformation is big, elastic restoration ratio is higher, excellent cementability and weatherability, can be used for high-rise building and fills out
The sealing of the concrete extension joint of facilities such as seam, large-sized concrete facility, road, bridge, airfield runway.The silicone of middle high-modulus
Fluid sealant is since its modulus is larger, tearing strength is low so that it is broken that it cohesion easily occurs after immersion, cold drawing hot pressing or immersion illumination
Bad or bonding interface destroys, and limits its application at larger displacement expansion joint.
Although low modulus silicone sealant have the advantages that it is so many, in the market still with the silicone sealant of middle high-modulus
Based on product.Chinese patent CN 104357005A《A kind of concrete road seam one-component silicone sealant and its preparation side
Method》A kind of low modulus one-component silicone sealant of road seam with low stretch modulus and good bonding provided,
For modulus all in 0.37~0.39MPa, the revision of the convention a to decimal is exactly 0.4MPa, is placed exactly in facing for low modulus and middle high-modulus
Dividing value.Chinese patent CN 106833503A《A kind of ketoxime removing type room temperature vulcanized silicone sealant of low modulus one-component and its preparation
Method》The low modulus silicone sealant of a kind of ketoxime removing type provided, although its modulus is met between 0.24~0.30MPa
The modulus requirement of low modulus fluid sealant, but surface drying speed is slower, it is undesirable in practical applications between 40~130min;
Although its a small amount of White Mineral Oil being added can play the role of reducing modulus, increase elongation, and White Mineral Oil dosage is also little,
But passing through the aging action of environment, White Mineral Oil can slowly ooze out fluid sealant, contaminated substrate.Chinese patent CN 1618915A《One
The low modulus silicone sealant of kind and its manufacturing method》A kind of low modulus silicone sealant provided, modulus 0.24~
Between 0.31MPa, 15~25min of surface drying time.Its methyl ethylene two used (epsilon-caprolactams base) silanes chain extender
With aminoxy silanes class crosslinking agent, although reactivity is high, source limits, is expensive, it is difficult to big in process of production
Amount uses.
Invention content
The present invention is the defect overcome described in the above-mentioned prior art, and it is weather-proof to provide a kind of low modR vulcanization neutral silicone
Fluid sealant, obtained silicone weatherproof sealant have lower modulus, excellent weather-resistant performance, good cementability and
Elastic restoration ratio.
Another object of the present invention is to provide the preparation sides that above-mentioned low modR vulcanizes neutral silicone weather proofing sealant
Method.
Another object of the present invention is to provide above-mentioned low modRs to vulcanize neutral silicone weather proofing sealant in Super High
The application in high displacement joint filling in building.
Another object of the present invention is to provide above-mentioned low modRs to vulcanize neutral silicone weather proofing sealant in road, bridge
Beam, airfield runway concrete extension joint sealing in application.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of low modR vulcanization neutral silicone weather proofing sealant, is grouped as by the group calculated by weight as follows:
The base polymer is that both ends are hydroxy-end capped dimethyl silicone polymer, 25 DEG C of the base polymer
At a temperature of viscosity be 60000~75000mPas;
Preferably, the powdered whiting and precipitated calcium carbonate weight ratio are 1~5:1.
Preferably, the average grain diameter of the precipitated calcium carbonate is 0.01~0.1 μm, the average grain diameter of the powdered whiting
It is 0.5~2 μm.
Preferably, the moisture content of the precipitated calcium carbonate and powdered whiting is less than or equal to 0.18%.
Preferably, the chain extender is two butanone oximino silane of diphenyl, two butanone oximino silane of aminomethyl phenyl, methyl second
Two butanone oximino silane of alkenyl, methyl ethylene dipropyl ketoximinosilanes, two butanone oximino silane of dimethyl, methyl ethylene two
One or more of acetoxylsilane.
Preferably, the coupling agent is vinyltriethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-shrink
Glycerine ether oxygen propyl trimethoxy silicane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-methacryloxypropyl
Base propyl trimethoxy silicane, three second of vinyl trimethoxysilane oligomer, vinyltriethoxysilane and γ-aminopropyl
Oligomer, γ-aminopropyltrimethoxysilane or its oligomer of oxysilane, gamma-aminopropyl-triethoxy-silane and γ-contracting
One or more of the oligomer of water glycerine ether oxygen propyl trimethoxy silicane.
Wherein, vinyltriethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl front three
Oxysilane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy silicon
Alkane, γ-aminopropyltrimethoxysilane are small molecule coupling agent.
Wherein, vinyl trimethoxysilane oligomer, vinyltriethoxysilane and gamma-aminopropyl-triethoxy silicon
Oligomer, γ-aminopropyltrimethoxysilane oligomer, gamma-aminopropyl-triethoxy-silane and the γ-glycidyl ether oxygen of alkane
The oligomer of propyl trimethoxy silicane is that small molecule coupling agent passes through oligomeric compound coupling agent obtained by the reaction.
Preferably, the coupling agent is vinyl trimethoxysilane oligomer, vinyltriethoxysilane and γ-ammonia
The oligomer of propyl-triethoxysilicane, γ-aminopropyltrimethoxysilane oligomer, gamma-aminopropyl-triethoxy-silane with
One or more of the oligomer of γ-glycidyl ether oxygen propyl trimethoxy silicane.
Preferably, viscosity of dimethicone at a temperature of 25 DEG C is 100~2000mm2/s。
Preferably, the crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, three butanone of propyl
Oximino silane, phenyl tributanoximo silane, four butanone oximino silanes, methyl tri acetylacetonate oximino silane, vinyl tri acetylacetonate oxime
One or more of base silane.
Preferably, the catalyst is dibutyl tin laurate, dibutyltin diacetate, stannous octoate, tin dilaurate
Dioctyl tin, dioctyl tin diacetate, two isooctyl acid tin of dibutyl, stannous 2-ethylhexoate, maleic acid list octanoic acid two are pungent
One or more of Ji Xi, ferric stearate, cobalt octoate, isooctyl acid bismuth, moon osmanthus Jiao acid bismuth, bismuth neodecanoate.
The present invention protects the preparation method of above-mentioned low modR vulcanization neutral silicone weather proofing sealant simultaneously, including as follows
Step:
S1. base polymer, dimethicone and chain extender are mixed at a temperature of 45~55 DEG C, add carbonic acid
Calcium, graphene oxide simultaneously stir dehydration, obtain base-material;
S2. the base-material of S1, crosslinking agent, coupling agent and catalyst are stirred evenly, the low neutral silicon of modR vulcanization is made
Ketone weather proofing sealant.
Preferably, the time being mixed in S1. is 20~30min.
Preferably, the condition that dehydration is stirred in S1. is the stirring dehydration in the case where 120 DEG C, vacuum degree are 0.08~0.1MPa
100~300min.
Preferably, to be stirred in planet kettle, it is 0.06~0.1MPa that the condition of stirring, which is in vacuum degree, for stirring in S2.,
30~80min is reacted under 200~800rpm of rotating speed.
The present invention also protects a high position of the above-mentioned low modR vulcanization neutral silicone weather proofing sealant in high-rise building
Move the application in joint filling.
The present invention also protects above-mentioned low modR to vulcanize neutral silicone weather proofing sealant in road, bridge, airfield runway
Concrete extension joint sealing in application.
Compared with prior art, the beneficial effects of the invention are as follows:
Low modR vulcanization neutral silicone weather proofing sealant provided by the invention is fully met《GB/T 22083-2008
Building sealant is classified and requires》With《GB/T 14683-2017 silicone and modified silicone building sealant》In+100/-50LM
Performance requirement, the silicone sealant have low stretch modulus, high resiliency and high elastic recovery rate and excellent weatherability and
Good adhesive property, after the processing such as cold drawing-hot pressing, immersion, be not in bonding interface destroy and cohesional failure, favorably
In the coagulation for promoting the facilities such as high displacement joint filling and road, bridge, airfield runway of the silicone sealant in high-rise building
The sealing at native expansion joint.
Specific implementation mode
Further illustrated the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.
The equal cocoa of raw material in embodiment is by being commercially available;
Unless stated otherwise, the present invention uses reagent, method and apparatus for the art conventional reagent, method and are set
It is standby.
In embodiment and comparative example,
In crosslinking agent, m (phenyl tributanoximo silane):M (vinyl tributyl ketoximyl silane)=1:2 mixture
It is by mass;M (phenyl tributanoximo silane):M (vinyl tributyl ketoximyl silane)=1:3 mixture, m (first
Base tributanoximo silane):M (vinyl tributyl ketoximyl silane)=3.5:1 mixture is equally by mass;
In coupling agent, m (vinyltrimethoxysilane):M (gamma-aminopropyl-triethoxy-silane)=1:1 it is oligomeric
Object, m (gamma-aminopropyl-triethoxy-silane):M (γ-glycidyl ether oxygen propyl trimethoxy silicane)=2:1 oligomer,
By mass.
Examples 1 to 5
Prepare low modR vulcanization neutral silicone weather proofing sealant:
The raw material usage amount of Examples 1 to 5 is as shown in table 1;
Reaction condition is as shown in table 2 in the preparation process of Examples 1 to 5;
Preparation process:
S1., base polymer, dimethicone and chain extender are mixed to t1 (min) at a temperature of T1 (DEG C), then added
Enter precipitated calcium carbonate, powdered whiting, graphene oxide in the case where T2 (DEG C), vacuum degree are P1 (MPa), stirring dehydration t2 (min),
Base-material is obtained after cooling;
S2. at room temperature, the base-material of S1. is added in planet stirring kettle, adds crosslinking agent, coupling agent and catalyst,
It is P2 (MPa) in vacuum degree, reacts t3 (min) under rotating speed r (rpm), it is neutral has both obtained the single-component room temperature vulcanized low modulus
Silicone weatherproof sealant.
Raw material usage amount (the unit of 1 Examples 1 to 5 of table:Part (weight))
Reaction condition in the preparation process of 2 Examples 1 to 5 of table
Performance test
Silicone sealant made from Examples 1 to 5 is carried out according to+100/-50 grades in GB/T 14683-2017 of requirement
Test;
The test result of silicone sealant made from Examples 1 to 5 is as shown in table 3;
The performance test results of 3 Examples 1 to 5 of table
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
All any modification, equivalent and improvement etc., should be included in the claims in the present invention made by within the spirit and principle of invention
Protection domain within.
Claims (10)
1. a kind of low modR vulcanizes neutral silicone weather proofing sealant, which is characterized in that by the group calculated by weight as follows
It is grouped as:
160 ~ 240 parts of base polymer;
30 ~ 80 parts of precipitated calcium carbonate;
100 ~ 160 parts of powdered whiting;
3 ~ 6 parts of graphene oxide;
12 ~ 30 parts of dimethicone;
8 ~ 15 parts of chain extender;
13 ~ 19 parts of crosslinking agent;
2.5 ~ 5 parts of coupling agent;
0.2 ~ 0.4 part of catalyst;
It is hydroxy-end capped dimethyl silicone polymer that the base polymer, which is both ends, at a temperature of 25 DEG C of the base polymer
Viscosity be 60000 ~ 75000mPas.
2. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the heavy
Calcium carbonate is 1 ~ 5 with precipitated calcium carbonate weight ratio:1.
3. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the lightweight
The average grain diameter of calcium carbonate is 0.01 ~ 0.1 μm, and the average grain diameter of the powdered whiting is 0.5 ~ 2 μm.
4. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the chain extension
Agent is two butanone oximino silane of diphenyl, two butanone oximino silane of aminomethyl phenyl, two butanone oximino silane of methyl ethylene, methyl
Vinyl dipropyl ketoximinosilanes, two butanone oximino silane of dimethyl, one kind in methyl ethylene diacetoxy silane or
It is several.
5. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the coupling
Agent is the oligomeric of vinyl trimethoxysilane oligomer, vinyltriethoxysilane and gamma-aminopropyl-triethoxy-silane
Object, γ-aminopropyltrimethoxysilane oligomer, gamma-aminopropyl-triethoxy-silane and γ-glycidyl ether oxygen propyl front three
One or more of oligomer of oxysilane.
6. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the diformazan
Viscosity of base silicone oil at a temperature of 25 DEG C is 100 ~ 2000mm2/s。
7. low modR according to claim 1 vulcanizes neutral silicone weather proofing sealant, which is characterized in that the crosslinking
Agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, propyl tributanoximo silane, three diacetylmonoxime of phenyl
One or more of base silane, four butanone oximino silanes, methyl tri acetylacetonate oximino silane, vinyl tri acetylacetonate oximino silane.
8. the preparation method of the low modR vulcanization neutral silicone weather proofing sealant of claim 1 ~ 7 any one of them, special
Sign is, includes the following steps:
S1. base polymer, dimethicone and chain extender are mixed at a temperature of 45 ~ 55 DEG C, add calcium carbonate,
Graphene oxide simultaneously stirs dehydration, obtains base-material;
S2. the base-material of S1, crosslinking agent, coupling agent and catalyst are stirred evenly, it is resistance to that low modR vulcanization neutral silicone is made
Wait fluid sealant.
9. the low modR of claim 1 ~ 7 any one of them vulcanizes neutral silicone weather proofing sealant in high-rise building
Application in high displacement joint filling.
10. the low modR of claim 1 ~ 7 any one of them vulcanizes neutral silicone weather proofing sealant in road, bridge, machine
Application in the sealing of the concrete extension joint of field runway.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115466504A (en) * | 2022-09-22 | 2022-12-13 | 中国电建集团成都勘测设计研究院有限公司 | Polyurethane for filling concrete expansion joint of hydraulic structure and preparation method thereof |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115466504A (en) * | 2022-09-22 | 2022-12-13 | 中国电建集团成都勘测设计研究院有限公司 | Polyurethane for filling concrete expansion joint of hydraulic structure and preparation method thereof |
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