CN108913087A - A kind of structural silicone adhesive and preparation method thereof of high intensity - Google Patents
A kind of structural silicone adhesive and preparation method thereof of high intensity Download PDFInfo
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- CN108913087A CN108913087A CN201810373846.8A CN201810373846A CN108913087A CN 108913087 A CN108913087 A CN 108913087A CN 201810373846 A CN201810373846 A CN 201810373846A CN 108913087 A CN108913087 A CN 108913087A
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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
-
- 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
-
- 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
-
- 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
- C08K2201/011—Nanostructured additives
-
- 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
-
- 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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides high-intensitive structural silicone adhesives, including following component according to parts by weight：40~50 parts of dialkyl polydimethylsiloxane, 5~10 parts of plasticizer, 40~50 parts of nanometer calcium carbonate, 2~8 parts of fumed silica, 5~7 parts of crosslinking agent, 0.7~0.8 part of coupling agent, 0.05~0.1 part of catalyst.The structural silicone adhesive of the invention has excellent mechanical property, it reaches 1.3MPa or more in room temperature (23 DEG C) Tensile strength, it is much higher by national regulations value 0.6MPa, and its tensile strength still with higher after immersion, reaches 1.28MPa or more.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of structural silicone adhesive of high intensity and its preparation side
Method.
Background technique
Structural silicone adhesive be a kind of one pack system, it is neutral solidify, aim at construction bonds assembly in building curtain wall and design,
It can squeeze out easily and use under very wide temperature condition, by the moisture-curing in air at excellent, durable high-modulus, height
The silicone rubber of elasticity.It is right since structure glue is that two or more material is tightly bonded together by glue
The intensity of structure glue itself and very high to the bonding force request of substrate；In the case where bonding force is constant, structure glue itself
Intensity it is bigger, it rise it is structural will be more stable.
And the structural silicone adhesive sold currently on the market mainly has SSG4000 and the Dow Corning Corporation of U.S. GE company
DC795, the tensile bond intensity of these products tensile bond intensity of especially soaking are all not ideal enough.Therefore, how by changing
Become the intensity that formula improves structure glue, is asking of needing to solve in building trade to meet the higher requirement of architectural decoration
Topic.
Summary of the invention
The purpose of the present invention is overcome the problems, such as that the tensile bond intensity of existing structural silicone adhesive is not ideal enough.
It is as follows including according to parts by weight for this purpose, the embodiment of the invention provides a kind of structural silicone adhesive of high intensity
Component：40~50 parts of dialkyl polydimethylsiloxane, 5~10 parts of plasticizer, 40~50 parts of nanometer calcium carbonate, gas phase titanium dioxide
2~8 parts of silicon, 5~7 parts of crosslinking agent, 0.7~0.8 part of coupling agent, 0.05~0.1 part of catalyst.
As one of embodiment, the viscosity of the dialkyl polydimethylsiloxane is 50000cps, and viscosity is too low,
Hardness is high after obtained structure glue vulcanization, poor flexibility, and its viscosity is excessively high, then the poor processability of structure glue.
As one of embodiment, the plasticizer is dimethyl silicone polymer.
As one of embodiment, the partial size of the nanometer calcium carbonate is 50~80nm.
As one of embodiment, the partial size of the fumed silica is 7~40nm, and specific surface is 150~200m2/
g。
As one of embodiment, the crosslinking agent is methyl tributanoximo silane and vinyl tributyl ketoximyl silane
Mixture, mass ratio 10:1.
As one of embodiment, the coupling agent is N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-ammonia
Any one of propyl-triethoxysilicane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane.
As one of embodiment, the catalyst is dibutyl tin dilaurate.
In addition, the embodiment of the invention also provides the preparation methods of the structural silicone adhesive of above-mentioned high intensity, including walk as follows
Suddenly：
1) dialkyl polydimethylsiloxane and plasticizer are added in high speed disperser by design proportion and are stirred evenly；
2) nanometer calcium carbonate is added in batches into high speed disperser, to the addition of nanometer calcium carbonate whole and after mixing evenly
Fumed silica is added, high-speed stirred is warming up to 100~125 DEG C, and vacuum -0.06~0.09MPa is dehydrated 2.5h, mills
It is cooling, obtain semi-finished product glue；
3) the semi-finished product glue that step 2) obtains is added in glue making machine, and the crosslinking agent by design proportion, coupling is added
Agent and catalyst, control temperature are no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get structural silicone adhesive.
Compared with prior art, beneficial effects of the present invention：The structural silicone adhesive of this high intensity provided by the invention is logical
It crosses and a small amount of fumed silica is added, small using its partial size, large specific surface area, superficial attractive forces are strong, the characteristic of good dispersion,
And make that structural silicone adhesive is with good stability, reinforcing and thickening property, and then substantially increase the intensity of silicone structure；
Structural silicone adhesive of the invention has excellent mechanical property, reaches 1.3MPa or more in room temperature (23 DEG C) Tensile strength,
It is much higher by national regulations value 0.6MPa, and its tensile strength still with higher after immersion, reaches 1.28MPa or more.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1：
The structural silicone adhesive for present embodiments providing a kind of high intensity, including following component according to parts by weight：Dihydroxy
40 parts of base dimethyl silicone polymer, 5 parts of plasticizer, 40 parts of nanometer calcium carbonate, 2 parts of fumed silica, 5 parts of crosslinking agent, coupling
0.7 part of agent, 0.1 part of catalyst；Wherein, the viscosity of dialkyl polydimethylsiloxane is 50000cps, and plasticizer selects poly- two
Methylsiloxane, the partial size of nanometer calcium carbonate are 80nm, and the partial size of fumed silica chooses 40nm, specific surface area 150m2/
G, crosslinking agent select methyl tributanoximo silane and vinyl tributyl ketoximyl silane in mass ratio 10:1 mixture, coupling
N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane is selected in agent, and catalyst selects dibutyl tin dilaurate.
The preparation method of the high-intensitive structural silicone adhesive of the embodiment, detailed process is as follows：
It is stirred firstly, dialkyl polydimethylsiloxane and plasticizer are weighed to be added in high speed disperser by above-mentioned quality
It mixes uniformly.
Then, nanometer calcium carbonate and fumed silica are weighed by above-mentioned quality, and nanometer calcium carbonate is divided into 4 times and is added
Enter into high speed disperser, be all added to nanometer calcium carbonate and add fumed silica, high-speed stirred after mixing evenly
100 DEG C are warming up to, vacuum -0.06~0.09MPa is dehydrated 2.5h, and cooling of milling obtains semi-finished product glue.
Finally, semi-finished product glue obtained above is added in glue making machine, and crosslinking agent, coupling agent are weighed by above-mentioned quality
It is added in glue making machine with catalyst, control temperature is no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get silicone
Structure glue.
Structural silicone adhesive made from the present embodiment is solidified at room temperature, observes its surface drying time；In polytetrafluoroethyl-ne
The structural silicone adhesive of one layer of 2mm thickness is uniformly applied on alkene plastics plate, room temperature curing 7 days, film is made, film is divided into 4 groups of progress
Test, 12~48h under the conditions of 4 groups of films are placed in 23 DEG C, 90 DEG C, -30 DEG C and are soaked respectively, then carry out tensile strength and fracture
The measurement of elongation, measurement result are as shown in table 1.
Embodiment 2：
The structural silicone adhesive for present embodiments providing a kind of high intensity, including following component according to parts by weight：Dihydroxy
42 parts of base dimethyl silicone polymer, 8 parts of plasticizer, 48 parts of nanometer calcium carbonate, 4 parts of fumed silica, 7 parts of crosslinking agent, coupling
0.8 part of agent, 0.08 part of catalyst；Wherein, the viscosity of dialkyl polydimethylsiloxane is 50000cps, and plasticizer selects poly- two
Methylsiloxane, the partial size of nanometer calcium carbonate are 80nm, and the partial size of fumed silica chooses 40nm, specific surface area 150m2/
G, crosslinking agent select methyl tributanoximo silane and vinyl tributyl ketoximyl silane in mass ratio 10:1 mixture, coupling
Gamma-aminopropyl-triethoxy-silane is selected in agent, and catalyst selects dibutyl tin dilaurate.
The preparation method of the high-intensitive structural silicone adhesive of the embodiment, detailed process is as follows：
It is stirred firstly, dialkyl polydimethylsiloxane and plasticizer are weighed to be added in high speed disperser by above-mentioned quality
It mixes uniformly.
Then, nanometer calcium carbonate and fumed silica are weighed by above-mentioned quality, and nanometer calcium carbonate is divided into 4 times and is added
Enter into high speed disperser, be all added to nanometer calcium carbonate and add fumed silica, high-speed stirred after mixing evenly
100 DEG C are warming up to, vacuum -0.06~0.09MPa is dehydrated 2.5h, and cooling of milling obtains semi-finished product glue.
Finally, semi-finished product glue obtained above is added in glue making machine, and crosslinking agent, coupling agent are weighed by above-mentioned quality
It is added in glue making machine with catalyst, control temperature is no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get silicone
Structure glue.
Structural silicone adhesive made from the present embodiment carries out the measurement of tensile strength and elongation at break, measurement result such as table
Shown in 1.
Embodiment 3：
The structural silicone adhesive for present embodiments providing a kind of high intensity, including following component according to parts by weight：Dihydroxy
45 parts of base dimethyl silicone polymer, 8 parts of plasticizer, 43 parts of nanometer calcium carbonate, 6 parts of fumed silica, 6 parts of crosslinking agent, coupling
0.7 part of agent, 0.07 part of catalyst；Wherein, the viscosity of dialkyl polydimethylsiloxane is 50000cps, and plasticizer selects poly- two
Methylsiloxane, the partial size of nanometer calcium carbonate are 50nm, and the partial size of fumed silica chooses 7nm, specific surface area 200m2/
G, crosslinking agent select methyl tributanoximo silane and vinyl tributyl ketoximyl silane in mass ratio 10:1 mixture, coupling
γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is selected in agent, and catalyst selects dibutyl tin dilaurate.
The preparation method of the high-intensitive structural silicone adhesive of the embodiment, detailed process is as follows：
It is stirred firstly, dialkyl polydimethylsiloxane and plasticizer are weighed to be added in high speed disperser by above-mentioned quality
It mixes uniformly.
Then, nanometer calcium carbonate and fumed silica are weighed by above-mentioned quality, and nanometer calcium carbonate is divided into 4 times and is added
Enter into high speed disperser, be all added to nanometer calcium carbonate and add fumed silica, high-speed stirred after mixing evenly
100 DEG C are warming up to, vacuum -0.06~0.09MPa is dehydrated 2.5h, and cooling of milling obtains semi-finished product glue.
Finally, semi-finished product glue obtained above is added in glue making machine, and crosslinking agent, coupling agent are weighed by above-mentioned quality
It is added in glue making machine with catalyst, control temperature is no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get silicone
Structure glue.
Structural silicone adhesive made from the present embodiment carries out the measurement of tensile strength and elongation at break, measurement result such as table
Shown in 1.
Embodiment 4：
The structural silicone adhesive for present embodiments providing a kind of high intensity, including following component according to parts by weight：Dihydroxy
50 parts of base dimethyl silicone polymer, 10 parts of plasticizer, 50 parts of nanometer calcium carbonate, 8 parts of fumed silica, 7 parts of crosslinking agent, coupling
0.8 part of agent, 0.05 part of catalyst；Wherein, the viscosity of dialkyl polydimethylsiloxane is 50000cps, and plasticizer selects poly- two
Methylsiloxane, the partial size of nanometer calcium carbonate are 80nm, and the partial size of fumed silica chooses 40nm, specific surface area 150m2/
G, crosslinking agent select methyl tributanoximo silane and vinyl tributyl ketoximyl silane in mass ratio 10:1 mixture, coupling
N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane is selected in agent, and catalyst selects dibutyl tin dilaurate.
The preparation method of the high-intensitive structural silicone adhesive of the embodiment, detailed process is as follows：
It is stirred firstly, dialkyl polydimethylsiloxane and plasticizer are weighed to be added in high speed disperser by above-mentioned quality
It mixes uniformly.
Then, nanometer calcium carbonate and fumed silica are weighed by above-mentioned quality, and nanometer calcium carbonate is divided into 4 times and is added
Enter into high speed disperser, be all added to nanometer calcium carbonate and add fumed silica, high-speed stirred after mixing evenly
100 DEG C are warming up to, vacuum -0.06~0.09MPa is dehydrated 2.5h, and cooling of milling obtains semi-finished product glue.
Finally, semi-finished product glue obtained above is added in glue making machine, and crosslinking agent, coupling agent are weighed by above-mentioned quality
It is added in glue making machine with catalyst, control temperature is no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get silicone
Structure glue.
Structural silicone adhesive made from the present embodiment carries out the measurement of tensile strength and elongation at break, measurement result such as table
Shown in 1.
Comparative example：
Structural silicone adhesive provided in this embodiment and preparation method thereof is the silicon of the present embodiment with embodiment 1, difference
Fumed silica is free of in ketone structure glue.
The structural silicone adhesive of the present embodiment is carried out to the measurement of tensile strength and elongation at break, measurement result such as table 1
It is shown.
Table 1：Structural silicone adhesive performance
As seen from Table 1, structural silicone adhesive produced by the present invention is greatly improved by the way that a small amount of fumed silica is added
The intensity of silicone structure, reaches 1.3MPa or more in room temperature (23 DEG C) Tensile strength, is much higher by national regulations value
0.6MPa, and its tensile strength still with higher after immersion, reach 1.28MPa or more.
The foregoing examples are only illustrative of the present invention, does not constitute the limitation to protection scope of the present invention, all
It is within being all belonged to the scope of protection of the present invention with the same or similar design of the present invention.
Claims (9)
1. a kind of structural silicone adhesive of high intensity, which is characterized in that including following component according to parts by weight：Dihydroxy poly- two
40~50 parts of methylsiloxane, 5~10 parts of plasticizer, 40~50 parts of nanometer calcium carbonate, 2~8 parts of fumed silica, crosslinking agent
5~7 parts, 0.7~0.8 part of coupling agent, 0.05~0.1 part of catalyst.
2. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the dialkyl polydimethylsiloxane
Viscosity be 50000cps.
3. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the plasticizer is polydimethylsiloxanes
Alkane.
4. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the partial size of the nanometer calcium carbonate is 50
~80nm.
5. structural silicone adhesive as described in claim 1 high-intensitive, which is characterized in that the partial size of the fumed silica is
7~40nm, specific surface are 150~200m2/g。
6. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the crosslinking agent is three diacetylmonoxime of methyl
The mixture of base silane and vinyl tributyl ketoximyl silane, mass ratio 10:1.
7. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the coupling agent is N- β-(ammonia second
Base)-γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy
Any one of silane.
8. high-intensitive structural silicone adhesive as described in claim 1, which is characterized in that the catalyst is two fourth of tin dilaurate
Ji Xi.
9. the preparation method of the structural silicone adhesive of high intensity as described in any one of claims 1 to 8, which is characterized in that including
Following steps：
1) dialkyl polydimethylsiloxane and plasticizer are added in high speed disperser by design proportion and are stirred evenly；
2) nanometer calcium carbonate is added in batches into high speed disperser, be all added to nanometer calcium carbonate and adds again after mixing evenly
Entering fumed silica, high-speed stirred is warming up to 100~125 DEG C, vacuum -0.06~0.09MPa, it is dehydrated 2.5h, cooling of milling,
Obtain semi-finished product glue；
3) the semi-finished product glue that step 2) obtains is added in glue making machine, and be added by the crosslinking agent of design proportion, coupling agent and
Catalyst, control temperature are no more than 50 DEG C, and vacuum -0.09MPa or more stirs 90min to get structural silicone adhesive.
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| CN201810373846.8A CN108913087A (en) | 2018-04-24 | 2018-04-24 | A kind of structural silicone adhesive and preparation method thereof of high intensity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110819296A (en) * | 2019-12-10 | 2020-02-21 | 佛山市高建硅胶实业有限公司 | Silicone weather-resistant sealant |
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| CN102382615A (en) * | 2010-09-03 | 2012-03-21 | 广州市白云化工实业有限公司 | Organosilicon sealant for solar photovoltaic modules and preparation method for organosilicon sealant |
-
2018
- 2018-04-24 CN CN201810373846.8A patent/CN108913087A/en active Pending
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|---|---|---|---|---|
| CN101353563A (en) * | 2008-09-11 | 2009-01-28 | 成都硅宝科技股份有限公司 | Single-component silicone fluid sealant for solar energy cell assembly and manufacturing method thereof |
| CN102382615A (en) * | 2010-09-03 | 2012-03-21 | 广州市白云化工实业有限公司 | Organosilicon sealant for solar photovoltaic modules and preparation method for organosilicon sealant |
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| CN110819296A (en) * | 2019-12-10 | 2020-02-21 | 佛山市高建硅胶实业有限公司 | Silicone weather-resistant sealant |
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