CN108977164A - A kind of room temperature vulcanization neutral silicone weather proofing sealant and its preparation method and application - Google Patents
A kind of room temperature vulcanization neutral silicone weather proofing sealant and its preparation method and application Download PDFInfo
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- CN108977164A CN108977164A CN201810511526.4A CN201810511526A CN108977164A CN 108977164 A CN108977164 A CN 108977164A CN 201810511526 A CN201810511526 A CN 201810511526A CN 108977164 A CN108977164 A CN 108977164A
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a kind of room temperature vulcanization neutral silicone weather proofing sealants, are 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 nitrogen-doped graphene；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, it is not in interfacial bonding destruction and cohesional failure, it may advantageously facilitate the sealing of the concrete extension joint of the high displacement facilities such as joint filling and road, bridge, airfield runway of the silicone sealant in super high-rise building.
Description
Technical field
The present invention relates to high molecule sealing materials technical fields, resistance to more particularly, to a kind of room temperature vulcanization neutral silicone
Wait sealant and its preparation method and application.
Background technique
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 achieve+100/-50, have
The advantages that permanent deformation is big, elastic restoration ratio is higher, excellent cementability and weatherability, can be used for super 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
Sealant is broken since its modulus is larger, tearing strength is low so that it cohesion easily occurs after immersion, cold drawing hot pressing or immersion illumination
Bad or interfacial bonding is destroyed, and limits it in the 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 " provide a kind of low modulus one-component silicone sealant of road seam with low stretch modulus and good bonding,
For modulus all in 0.37~0.39MPa, the revision of the convention a to decimal is exactly 0.4MPa, is placed exactly in the critical of low modulus and middle high-modulus
Value.Chinese patent CN 106833503A " a kind of ketoxime removing type room temperature vulcanized silicone sealant of low modulus one-component and its preparation side
Method " provide a kind of low modulus silicone sealant of ketoxime removing type, although its modulus between 0.24~0.30MPa, is met low
The modulus requirement of modulus sealant, but surface drying speed is slower, it is undesirable in practical applications between 40~130min；Though
So 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
It is the aging action by environment, White Mineral Oil can slowly ooze out sealant, contaminated substrate.Chinese patent CN 1618915A is " a kind of
Low modulus silicone sealant and its manufacturing method " provide a kind of low modulus silicone sealant, modulus is in 0.24~0.31MPa
Between, 15~25min of surface drying time.Its methyl ethylene two used (epsilon-caprolactams base) silanes chain extender and aminooxy group
Silane-type cross-linking agent, although reactivity is high, source limits, is expensive, is difficult largely to use in process of production.
Summary of the invention
The present invention is to overcome defect described in the above-mentioned prior art, provides a kind of weather-proof sealing of room temperature vulcanization neutral silicone
Glue, obtained silicone weatherproof sealant have lower modulus, excellent weather-resistant performance, good cementability and elasticity
Recovery rate.
Another object of the present invention is to provide the preparation methods of above-mentioned room temperature vulcanization neutral silicone weather proofing sealant.
Another object of the present invention is to provide above-mentioned room temperature vulcanization neutral silicone weather proofing sealants in super high-rise building
High displacement joint filling in application.
Another object of the present invention is to provide above-mentioned room temperature vulcanization neutral silicone weather proofing sealants in road, bridge, machine
Application in the sealing of the concrete extension joint of field runway.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of room temperature 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 temperature of the base polymer
Viscosity under degree is 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 that vinyltriethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-shrink are sweet
Oily ether oxygen propyl trimethoxy silicane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-methacryloxy third
Base trimethoxy silane, vinyl trimethoxysilane oligomer, vinyltriethoxysilane and gamma-aminopropyl-triethoxy
Oligomer, γ-aminopropyltrimethoxysilane or its oligomer of silane, gamma-aminopropyl-triethoxy-silane and γ-shrink are sweet
One or more of the oligomer of oily 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 the oligomeric compound coupling agent that small molecule coupling agent is obtained by 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 γ-glycidyl ether oxygen propyl trimethoxy silicane oligomer.
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 dilaurate, 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 also protects the preparation method of above-mentioned room temperature vulcanization neutral silicone weather proofing sealant, includes the following steps:
S1. base polymer, dimethicone and chain extender are mixed at a temperature of 45~55 DEG C, add carbonic acid
Calcium, nitrogen-doped graphene simultaneously stir dehydration, obtain base-material；
S2. the base-material of S1, crosslinking agent, coupling agent and catalyst are stirred evenly, it is weather-proof that room temperature vulcanization neutral silicone is made
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 stir 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 revolving speed.
The present invention protects high displacement of the above-mentioned room temperature vulcanization neutral silicone weather proofing sealant in super high-rise building to fill out simultaneously
Application in seam.
The present invention also protect above-mentioned room temperature vulcanization neutral silicone weather proofing sealant road, bridge, airfield runway coagulation
Application in the sealing at native expansion joint.
Compared with prior art, the beneficial effects of the present invention are:
Room temperature vulcanization neutral silicone weather proofing sealant provided by the invention fully meet " GB/T 22083-2008 building it is close
Sealing classification and require " and " GB/T 14683-2017 silicone and modified silicone building sealant " in+100/-50LM performance
It is required that the silicone sealant has low stretch modulus, high resiliency and high elastic recovery rate and excellent weatherability and good
Adhesive property is not in interfacial bonding destruction and cohesional failure, may advantageously facilitate after the processing such as cold drawing-hot pressing, immersion
The concrete of the high displacement facilities such as joint filling and road, bridge, airfield runway of the silicone sealant in super high-rise building is flexible
The sealing of seam.
Specific embodiment
Further illustrate 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 is
By mass；M (phenyl tributanoximo silane): m (vinyl tributyl ketoximyl silane)=1:3 mixture, m (methyl
Tributanoximo silane): m (vinyl tributyl ketoximyl silane)=3.5:1 mixture, is equally by mass；
In coupling agent, the oligomer of m (vinyltrimethoxysilane): m (gamma-aminopropyl-triethoxy-silane)=1:1,
The oligomer of m (gamma-aminopropyl-triethoxy-silane): m (γ-glycidyl ether oxygen propyl trimethoxy silicane)=2:1, is pressed
Mass Calculation.
Examples 1 to 5
Prepare room temperature 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 step of Examples 1 to 5；
Preparation step:
S1., base polymer, dimethicone and chain extender be mixed to t1 (min) at a temperature of T1 (DEG C), then plus
Enter precipitated calcium carbonate, powdered whiting, nitrogen-doped graphene 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 revolving speed r (rpm), it is neutral has both obtained the single-component room temperature vulcanized low modulus
Silicone weatherproof sealant.
The raw material usage amount (unit: part (weight)) of 1 Examples 1 to 5 of table
Reaction condition in the preparation step 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
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of room temperature vulcanization neutral silicone weather proofing sealant, which is characterized in that be 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 nitrogen-doped graphene；
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, at a temperature of 25 DEG C of the base polymer
Viscosity be 60000 ~ 75000mPas.
2. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the powdered whiting
It is 1 ~ 5:1 with precipitated calcium carbonate weight ratio.
3. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the precipitated calcium carbonate
Average grain diameter be 0.01 ~ 0.1 μm, the average grain diameter of the powdered whiting is 0.5 ~ 2 μm.
4. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the chain extender is two
Two butanone oximino silane of phenyl, two butanone oximino silane of aminomethyl phenyl, two butanone oximino silane of methyl ethylene, methyl ethylene
One or more of dipropyl ketoximinosilanes, two butanone oximino silane of dimethyl, methyl ethylene diacetoxy silane.
5. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the coupling agent is second
Alkenyl trimethoxysilane oligomer, the oligomer of vinyltriethoxysilane and gamma-aminopropyl-triethoxy-silane, γ-
Aminopropyl trimethoxysilane oligomer, gamma-aminopropyl-triethoxy-silane and γ-glycidyl ether oxygen propyl trimethoxy silicon
One or more of oligomer of alkane.
6. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the dimethicone
Viscosity at a temperature of 25 DEG C is 100 ~ 2000mm2/s。
7. room temperature vulcanization neutral silicone weather proofing sealant according to claim 1, which is characterized in that the crosslinking agent is first
Base tributanoximo silane, vinyl tributyl ketoximyl silane, propyl tributanoximo silane, phenyl tributanoximo silane,
One or more of four butanone oximino silanes, methyl tri acetylacetonate oximino silane, vinyl tri acetylacetonate oximino silane.
8. the preparation method of the described in any item room temperature vulcanization neutral silicone weather proofing sealants of claim 1 ~ 7, which is characterized in that
Include the following steps:
S1. base polymer, dimethicone and chain extender are mixed at a temperature of 45 ~ 55 DEG C, add calcium carbonate,
Nitrogen-doped graphene simultaneously stirs dehydration, obtains base-material；
S2. the base-material of S1, crosslinking agent, coupling agent and catalyst are stirred evenly, the weather-proof sealing of room temperature vulcanization neutral silicone is made
Glue.
9. high displacement of the described in any item room temperature vulcanization neutral silicone weather proofing sealants of claim 1 ~ 7 in super high-rise building
Application in joint filling.
10. the described in any item room temperature vulcanization neutral silicone weather proofing sealants of claim 1 ~ 7 are in road, bridge, airfield runway
Concrete extension joint sealing in application.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810511526.4A CN108977164A (en) | 2018-05-24 | 2018-05-24 | A kind of room temperature vulcanization neutral silicone weather proofing sealant and its preparation method and application |
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| CN201810511526.4A CN108977164A (en) | 2018-05-24 | 2018-05-24 | A kind of room temperature vulcanization neutral silicone weather proofing sealant and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694686A (en) * | 2018-12-27 | 2019-04-30 | 广州市白云化工实业有限公司 | Single-component silicone fluid sealant and preparation method thereof |
| CN113265221A (en) * | 2021-04-30 | 2021-08-17 | 广州绿腾新材料有限公司 | Silicone sealant with anti-bulging performance and preparation method thereof |
-
2018
- 2018-05-24 CN CN201810511526.4A patent/CN108977164A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694686A (en) * | 2018-12-27 | 2019-04-30 | 广州市白云化工实业有限公司 | Single-component silicone fluid sealant and preparation method thereof |
| CN113265221A (en) * | 2021-04-30 | 2021-08-17 | 广州绿腾新材料有限公司 | Silicone sealant with anti-bulging performance and preparation method thereof |
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Application publication date: 20181211 |