CN112210341A - Double-vulcanization system building sealant and preparation method thereof - Google Patents
Double-vulcanization system building sealant and preparation method thereof Download PDFInfo
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- CN112210341A CN112210341A CN202010988854.0A CN202010988854A CN112210341A CN 112210341 A CN112210341 A CN 112210341A CN 202010988854 A CN202010988854 A CN 202010988854A CN 112210341 A CN112210341 A CN 112210341A
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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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C08K2201/011—Nanostructured additives
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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
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a double-vulcanization system building sealant and a preparation method thereof, belonging to the technical field of building sealants. The double-vulcanization system building sealant comprises a component A and a component B, wherein the component A comprises the following components: (a) 500-540 parts of alkoxy-terminated vinyl-containing 107 glue, (b) 40-60 parts of dimeticone, (c) 50-70 parts of white oil, (d) 1000 parts of calcium carbonate 950-; and B component: (f) 25-55 parts of alkoxy silane cross-linking agent containing silicon hydride, (g) 28-30 parts of titanium catalyst, (h) 3.0-3.4 parts of organic silicon coupling agent. The double-vulcanization system building sealant disclosed by the invention is high in curing speed, capable of being cured deeply, strong in binding power and excellent in yellowing resistance; the invention also provides a simple and feasible preparation method.
Description
Technical Field
The invention relates to a double-vulcanization system building sealant and a preparation method thereof, belonging to the technical field of building sealants.
Background
The dealcoholized silicone building sealant is divided into a single-component dealcoholized building sealant and a double-component dealcoholized building sealant, has low odor, no corrosion, environmental protection and good caking property to glass, metal and most base materials. With the rapid development of industries such as electronic and electric products, automobile transportation, civil engineering and construction and the like and the higher and higher requirements on environmental protection, the dealcoholized silicone adhesive has higher and higher demand, and becomes an important project for the research of sealant enterprises.
At present, the dealcoholized sealant in the domestic market still has some defects, such as deep curing problem, no matter the sealant is a double-component sealant or a single-component sealant, deep curing is carried out from the surface to the inside by means of moisture, such as moisture of air, so that the deep curing is not thorough, the construction period is long, the construction thickness exceeds a certain thickness, the inside is difficult to cure, and the bonding firmness with a base material is influenced.
In addition, the sizing material is easy to yellow, and the alcohol type transparent adhesive produced by adopting alkoxy end capping 107, a stabilizing agent, an organic tin chelate, fumed silica, a coupling agent and the like has yellow colloid because the end capping agent, the chelating agent, the introduced coupling agent and the like contain yellow functional groups.
Therefore, the dealcoholized building sealant with the double-vulcanization system, which has the advantages of high curing speed, deep curing, excellent yellowing resistance and strong bonding force, is developed, and has wide application prospect.
Disclosure of Invention
The invention aims to solve the technical problems that the defects in the prior art are overcome, and the dual-vulcanization system building sealant is provided, has high curing speed, deep curing capability and strong bonding force, and also has excellent yellowing resistance; the invention also provides a simple and feasible preparation method.
The double-vulcanization system building sealant comprises a component A and a component B,
the component A comprises the following raw materials in parts by mass:
the component B comprises the following raw materials in parts by mass:
(f) 25-55 parts of alkoxy silane crosslinking agent containing silicon hydride
(g) 28-30 parts of titanium catalyst
(h) 3.0-3.4 parts of organosilicon coupling agent.
Preferably, the molecular weight of the alkoxy-terminated vinyl-containing 107 glue is 2-50 ten thousand, the mass content of the vinyl is 0.01% -3.0%, and the molecular formula is as follows: vi (CH)3O)2SiO[(CH3)2SiO]m[Vi(CH3)SiO]nSi(OCH3)2Vi。
The molecular chain of the alkoxy-terminated vinyl-containing 107 glue must contain both vinyl and methoxy groups, wherein the end parts are blocked by two methoxy groups and one vinyl group, and the middle part of the chain must contain the vinyl group.
Preferably, the alkoxy-terminated vinyl-containing 107 adhesive has a viscosity of 8 ten thousand and a vinyl content of 0.16% by mass.
Preferably, the dimethicone has a viscosity of < 350 cs.
Preferably, the white oil is a commercially available # 3 white oil.
The calcium carbonate is commercially available nano calcium carbonate.
The alkoxy silane cross-linking agent containing silicon hydride has a molecular formula of (CH)3O)2SiH(CH3) F1 or of methyltrimethoxysilane and hydrogen-containing silicone oilThe mixture f2 and f1 contains methoxyl and silicon hydrogen bonds in molecules. Preferably, the amount of f1 is 30-50 parts by mass, the amount of methyltrimethoxysilane is 20-40 parts by mass, and the amount of hydrogen-containing silicone oil is 5-15 parts by mass.
Preferably, the titanium catalyst is commercially available isopropyl teraphthalate, isobutyl teraphthalate or a titanium complex.
Preferably, the silicone coupling agent is KH550, KH560 or KH792, more preferably γ -aminopropyltriethoxysilane.
The preparation method of the double-vulcanization system building sealant comprises the following steps:
(1) the component A is uniformly mixed at room temperature according to the proportion, and is vacuumized and sealed for storage in a sealed manner in the whole process;
(2) uniformly mixing the component B at room temperature according to the proportion, vacuumizing the whole process, and sealing and storing;
(3) when in use, the component A and the component B are mixed evenly and used in time within 4 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the designed dealcoholized building sealant formula, a double vulcanization system is used, the double vulcanization system has the functions of two vulcanization systems, small molecules can be removed from outside to inside by means of moisture in the air for curing, and hydrosilylation can be performed under the action of a platinum catalyst to perform deep curing; the concrete can be formed on site during construction, is convenient to use, can be deeply cured, and has no requirement on construction thickness;
(2) the dealcoholized building sealant formula of the double-vulcanization system contains silicon-hydrogen bonds which are relatively active and can be used as an anti-yellowing agent with excellent performance, so that the sealant is endowed with good yellowing resistance;
(3) in the designed dealcoholized building sealant formula, a double-vulcanization system is used, so that the adhesive tape is easier to have tensile strength in a short time, and the adhesion with a base material is improved in a short time;
(4) the titanium catalyst and the platinum catalyst are both nontoxic and pollution-free catalysts and have environmental protection property;
(5) the preparation method is simple and feasible, and is beneficial to industrial production.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
In the Kansted catalyst used in the examples, the platinum content by mass was 5000 ppm.
Example 1
The dealcoholized building sealant silicone rubber with the double-vulcanization system comprises the following raw materials in parts by mass:
and (B) glue component A:
(a) 520 parts of 107 glue containing alkoxy end-capped vinyl
(b) 50 portions of dimeticone (the viscosity is less than 350cs)
(c) 60 portions of white oil
(d) 975 parts of calcium carbonate
(e) 3 parts of a Kaster catalyst;
b, glue component:
(f1) 40 parts of alkoxy silane containing silicon hydride
(g) Titanium catalyst 29 parts
(h) KH 5503.2 parts.
The preparation steps of the glue A are as follows:
according to the following proportion, (a) 520 parts of 107 glue containing vinyl and terminated by alkoxy, (b) 50 parts of dimeticone (the viscosity is less than 350cs), (c) 60 parts of white oil, (d) 975 parts of calcium carbonate powder, (e) 3 parts of Kanster catalyst are uniformly mixed in a planetary mixer, the vacuum degree is-0.05 MPa, the mixing temperature is not more than 60 ℃, and after uniform mixing, circulating water cooling is needed to be introduced to obtain glue A;
the preparation steps of the B glue are as follows:
40 parts of an alkoxysilane containing hydrosilation, (f1), 29 parts of a titanium catalyst, and (h) KH 5503.2. Mixing in a planetary mixer under vacuum degree of-0.05 MPa and mixing temperature not higher than 60 deg.C, cooling with circulating water to obtain glue B;
and uniformly mixing the component A and the component B in vacuum, and testing.
Example 2
The dealcoholized building sealant silicone rubber with the double-vulcanization system comprises the following raw materials in parts by mass:
and (B) glue component A:
(a) 520 parts of 107 glue containing alkoxy end-capped vinyl
(b) 50 portions of dimeticone (the viscosity is less than 350cs)
(c) 60 portions of white oil
(d) 975 parts of calcium carbonate
(e) 3 parts of a platinum catalyst;
b, glue component:
(f2) mixture of 30 parts of methyltrimethoxysilane and 10 parts of hydrogen-containing silicone oil
(g) Titanium catalyst 29 parts
(h) KH 5503.2 parts.
The preparation steps of the glue A are as follows:
according to the following proportion, (a) 520 parts of 107 glue containing vinyl and terminated by alkoxy, (b) 50 parts of dimeticone (the viscosity is less than 350cs), (c) 60 parts of white oil, (d) 975 parts of calcium carbonate powder, (e) 3 parts of platinum catalyst, 5000ppm are uniformly mixed in a planetary mixer, the vacuum degree is-0.1 MPa, the mixing temperature is not more than 60 ℃, and after uniform mixing, circulating water is needed to be introduced for cooling, thus obtaining glue A;
the preparation steps of the B glue are as follows:
according to the following proportions, (f2) 30 parts of methyltrimethoxysilane and 10 parts of hydrogen-containing silicone oil, (g) 29 parts of titanium catalyst, and (h) KH 5503.2 parts. Mixing in a planetary mixer under vacuum degree of-0.1 MPa and mixing temperature not higher than 60 deg.C, cooling with circulating water to obtain glue B;
and uniformly mixing the component A and the component B in vacuum, and testing.
Example 3
The dealcoholized building sealant silicone rubber with the double-vulcanization system comprises the following raw materials in parts by mass:
and (B) glue component A:
(a) 500 parts of 107 adhesive with alkoxy end capping and vinyl
(b) 40 portions of dimeticone (the viscosity is less than 350cs)
(c) 50 portions of white oil
(d) 950 parts of calcium carbonate
(e) 2 parts of a Kaster catalyst;
b, glue component:
(f1) 30 parts of alkoxy silane containing silicon hydride
(g) Titanium catalyst 28 parts
(h) KH 5503.0 parts.
The preparation steps of the glue A are as follows:
according to the following proportions, (a) 500 parts of alkoxy-terminated vinyl-containing 107 glue, (b) 40 parts of simethicone (the viscosity is less than 350cs), (c) 50 parts of white oil, (d) 950 parts of calcium carbonate powder, (e) 2 parts of Kanster catalyst are uniformly mixed in a planetary mixer, the vacuum degree is-0.05 MPa, the mixing temperature is not more than 60 ℃, and after uniform mixing, circulating water is needed to be introduced for cooling, so that glue A is obtained;
the preparation steps of the B glue are as follows:
according to the following proportions, (f1) 30 parts of hydrosilyl-containing alkoxysilane, (g) 28 parts of titanium catalyst, and (h) KH 5503.0 parts. Mixing in a planetary mixer under vacuum degree of-0.05 MPa and mixing temperature not higher than 60 deg.C, cooling with circulating water to obtain glue B;
and uniformly mixing the component A and the component B in vacuum, and testing.
Example 4
The dealcoholized building sealant silicone rubber with the double-vulcanization system comprises the following raw materials in parts by mass:
and (B) glue component A:
(a) 540 parts of 107 glue containing alkoxy end-capped vinyl
(b) 60 portions of dimeticone (the viscosity is less than 350cs)
(c) 70 portions of white oil
(d) 1000 parts of calcium carbonate
(e) 4 parts of a Kaster catalyst;
b, glue component:
(f2) 40 parts of methyltrimethoxysilane and 15 parts of hydrogen-containing silicone oil
(g) Titanium catalyst 30 parts
(h) KH 5503.4 parts.
The preparation steps of the glue A are as follows:
540 parts of 107 glue containing vinyl and terminated by alkoxy, (b) 60 parts of dimeticone (the viscosity is less than 350cs), (c) 70 parts of white oil, (d) 1000 parts of calcium carbonate, (e) 4 parts of Kanster catalyst are uniformly mixed in a planetary mixer, the vacuum degree is-0.05 MPa, the mixing temperature is not more than 60 ℃, and after uniform mixing, circulating water is introduced for cooling to obtain glue A;
the preparation steps of the B glue are as follows:
40 parts of methyltrimethoxysilane (f2), 15 parts of hydrogen-containing silicone oil (g), 30 parts of titanium catalyst and (h) KH 5503.4. Mixing in a planetary mixer under vacuum degree of-0.05 MPa and mixing temperature not higher than 60 deg.C, cooling with circulating water to obtain glue B;
and uniformly mixing the component A and the component B in vacuum, and testing.
Comparative example 1
The single-vulcanization system dealcoholized building sealant silicone rubber comprises the following raw materials in parts by mass:
and (B) glue component A:
(1) 520 parts of 107 adhesive with alkoxy end capping
(2) 50 portions of dimeticone (the viscosity is less than 350cs)
(3) 60 portions of white oil
(4) 975 parts of calcium carbonate;
b, glue component:
(11) 40 parts of methyltrimethoxysilane
(22) Titanium catalyst 29 parts
(33) KH 5503.2 parts
(44) 5 parts of organic tin catalyst.
The preparation steps of the glue A are as follows:
according to the following proportion, (1) 520 parts of 107 glue with end capped by alkoxy, (2) 50 parts of dimeticone (the viscosity is less than 350cs), (3) 60 parts of white oil, and (4) 975 parts of calcium carbonate powder are uniformly mixed in a planetary mixer, the vacuum degree is-0.05 MPa to-0.1 MPa, the mixing temperature is not more than 60 ℃, and after uniform mixing, circulating water is needed to be introduced for cooling, thus obtaining glue A;
the preparation steps of the B glue are as follows:
40 parts of methyltrimethoxysilane (11), 29 parts of titanium catalyst (22), 33 parts of KH 5503.2 parts and 5 parts of organotin catalyst (44) according to the following proportions. Mixing in a planetary mixer under vacuum degree of-0.05 MPa and mixing temperature not higher than 60 deg.C, cooling with circulating water to obtain glue B;
and uniformly mixing the component A and the component B in vacuum, and testing.
Examples 1-4 and comparative example 1 were tested and the results are shown in table 1.
TABLE 1
As shown by comparing the test results of example 1, example 2, example 3, example 4 and comparative example 1 in Table 1, examples 1 and 2 obtained an environmentally friendly dealcoholized building sealant of a two-vulcanization system having a high curing speed, deep curing, excellent yellowing resistance and strong adhesion.
Claims (8)
1. The double-vulcanization system building sealant comprises a component A and a component B, and is characterized in that:
the component A comprises the following raw materials in parts by mass:
the component B comprises the following raw materials in parts by mass:
(f) 25-55 parts of alkoxy silane crosslinking agent containing silicon hydride
(g) 28-30 parts of titanium catalyst
(h) 3.0-3.4 parts of organosilicon coupling agent.
2. The dual cure system building sealant according to claim 1, wherein: the molecular weight of the alkoxy-terminated vinyl-containing 107 glue is 2-50 ten thousand, the mass content of the vinyl is 0.01-3.0%, and the molecular formula is as follows: vi (CH)3O)2SiO[(CH3)2SiO]m[Vi(CH3)SiO]nSi(OCH3)2Vi。
3. The dual cure system building sealant according to claim 1, wherein: the molecular chain of the alkoxy-terminated vinyl-containing 107 glue simultaneously contains vinyl and methoxyl, wherein the end parts are terminated by two methoxyl and one vinyl, and the middle part of the chain contains the vinyl.
4. The dual cure system building sealant according to claim 1, wherein: the alkoxy-terminated vinyl group-containing 107 had a viscosity of 8 ten thousand and a vinyl group content of 0.16% by mass.
5. The dual cure system building sealant according to claim 1, wherein: the viscosity of the simethicone is less than 350 cs.
6. The dual cure system building sealant according to claim 1, wherein: the alkoxysilane crosslinking agent containing hydrosilation has a molecular formula of (CH)3O)2SiH(CH3) Or f1 is a mixture of methyltrimethoxysilane and hydrogen-containing silicone oil f2, and f1 molecules simultaneously contain methoxyl and silicon hydrogen bonds.
7. The dual cure system building sealant according to claim 1, wherein: the titanium catalyst is isopropyl teraphthalate, isobutyl teraphthalate or a titanium complex.
8. A method of preparing the dual cure system building sealant according to any one of claims 1 to 7, wherein: the method comprises the following steps:
(1) the component A is uniformly mixed at room temperature according to the proportion, and is vacuumized and sealed for storage in a sealed manner in the whole process;
(2) uniformly mixing the component B at room temperature according to the proportion, vacuumizing the whole process, and sealing and storing;
(3) when in use, the component A and the component B are mixed evenly and used in time within 4 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185546A (en) * | 2021-04-28 | 2021-07-30 | 广州市白云化工实业有限公司 | High-activity catalyst for dealcoholized silicone sealant and preparation method and application thereof |
| CN115418192A (en) * | 2022-10-15 | 2022-12-02 | 江苏矽时代材料科技有限公司 | Addition type room temperature curing high-bonding-strength pouring sealant and preparation method and application thereof |
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