CN109337631B - Preparation method of silane-terminated sealant with excellent medium resistance - Google Patents
Preparation method of silane-terminated sealant with excellent medium resistance Download PDFInfo
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- CN109337631B CN109337631B CN201811233112.6A CN201811233112A CN109337631B CN 109337631 B CN109337631 B CN 109337631B CN 201811233112 A CN201811233112 A CN 201811233112A CN 109337631 B CN109337631 B CN 109337631B
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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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
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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
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a preparation method of a silane-terminated sealant with excellent medium resistance, which comprises the following steps: adding the silyl-terminated polyether, the plasticizer, the pretreated filler, the pigment, the antioxidant, the ultraviolet light absorber and the light stabilizer into a double-planet stirring kettle in sequence, stirring and dispersing at 100-110 ℃, dehydrating in vacuum for 2 hours under the condition that the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding the water removing agent into the double-planet stirring kettle, mixing for 30 minutes under the vacuum state, adding the tackifier and the catalyst into the stirring kettle, mixing for 10 minutes under the vacuum state, and adding N2Sealing and packaging. The silane-terminated sealant with excellent medium resistance provided by the invention is packaged in a single component manner, is easy to glue, has higher adhesive force to various base materials after being cured, has high adhesive strength retention rate after being soaked in engine oil, and can well meet the safe use requirements of industries such as automobiles, locomotives and the like.
Description
Technical Field
The invention relates to a preparation method of a silane-terminated sealant with excellent medium resistance, in particular to a preparation method of a silane-modified polyether sealant with engine oil resistance and strong bonding force.
Background
The silyl-terminated polyether type elastic sealant is also called organosilicon modified polyether sealant, modified silicone sealant and MS sealant. It originates from japan and has a great number of applications in the construction industry. The adhesive has the characteristics of paintability, good bonding force to most base materials, no solvent and the like, has more applications in two or three years, can partially replace silicone sealant or polyurethane adhesive in some occasions, and is applied to the fields of automobiles, locomotives and the like.
Disclosure of Invention
The invention provides a preparation method of a silane-terminated sealant with excellent medium resistance, and the prepared sealant has excellent engine oil resistance, has good adhesion on most base materials, and can well meet the reliability requirement of a product in the using process.
The invention relates to a preparation method of a silane-terminated sealant with excellent medium resistance, which comprises the following steps:
(1) pretreatment of the filler: adding a filler into a stirring kettle, heating while stirring, adding a coupling agent gamma-glycidyl ether oxy propyl trimethoxy silane KH560 with the dosage of 0.3 percent of the total amount of the filler and a coupling agent A174[ gamma- (methacryloyloxy) propyl trimethoxy silane ] with the dosage of 0.6 percent of the total amount of the filler when the temperature is raised to 150 ℃, keeping the temperature at 150 ℃, vacuumizing for 3 hours, closing heating, maintaining the pressure, naturally cooling or discharging the mixture after cooling by circulating water for later use;
(2) Sequentially adding 25-45 parts of silyl-terminated polyether, 10-20 parts of plasticizer, 25-45 parts of filler in the step (1), 1-10 parts of pigment, 1-2 parts of antioxidant, 1-2 parts of ultraviolet absorber and 1-2 parts of light stabilizer into a double-planetary stirring kettle, stirring and dispersing at 100-110 ℃ and carrying out vacuum dehydration for 2 hours, wherein the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding 1-5 parts of water removing agent into the double-planetary stirring kettle, mixing for 30 minutes in a vacuum state, adding 1-5 parts of tackifier into the stirring kettle, mixing for 10 minutes in a vacuum state, finally adding 0.5-2 parts of catalyst into the stirring kettle, mixing for 10 minutes in a vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is not less than-0.098 MPa2Sealing and packaging.
The pretreatment of the filler increases the medium resistance and the sedimentation resistance of the filler, and on the basis of the technical scheme, the invention can be further improved as follows.
Further, the end-silane polyether is one or a mixture of more of MAX923, MAX951, MAX602 and SAX530 of KANEKA in Japan.
The beneficial effects of using these several silane-terminated polyethers are: the acrylic acid modified silyl-terminated polyether is adopted, and after acrylic acid is introduced into a chain segment, the polarity of a polymer is increased, and the engine oil resistance of the sealant is improved.
Further, the plasticizer is diisononyl phthalate (DINP), diisodecyl phthalate (DIDP), SAT010 of KANEKA in Japan.
Further, the filler is one or a mixture of several of nano active calcium carbonate, silicon micropowder and gas-phase silicon dioxide.
Further, the pigment is one of titanium dioxide and carbon black.
Further, the antioxidant is one of an antioxidant 1010 and an antioxidant 1076.
Further, the light stabilizer is bis (2, 2, 6, 6-tetramethyl-4-piperidyl) sebacate.
Further, the ultraviolet absorber is 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole.
Further, the water removing agent is vinyl trimethoxy silane.
Further, the tackifier is one or a mixture of more of N-beta-aminoethyl-gamma-aminopropyltrimethoxysilane, aminopropyltrimethoxysilane and aminopropyltriethoxysilane.
Further, the catalyst is one or a mixture of more of U-220H, U-303 and stannous octoate formed by chemical reaction in the east China.
The invention has the beneficial effects that: the silane-terminated sealant with excellent medium resistance provided by the invention is packaged in a single component manner, is easy to glue, has higher adhesive force to various base materials after being cured, has high adhesive strength retention rate after being soaked in engine oil, and can well meet the safe use requirements of industries such as automobiles, locomotives and the like.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Pretreatment of the filler: adding a filler into a stirring kettle, heating while stirring, adding a coupling agent KH560 (gamma-glycidyl ether oxypropyltrimethoxysilane) in an amount of 0.3 percent of the total amount of the filler and a coupling agent A174[ gamma- (methacryloyloxy) propyl trimethoxysilane ] in an amount of 0.6 percent of the total amount of the filler when the temperature is raised to 150 ℃, keeping the temperature at 150 ℃, vacuumizing for 3 hours, closing heating, maintaining the pressure, naturally cooling or cooling by circulating water and discharging for later use, wherein all the nano active calcium carbonate, the silicon micropowder and the fumed silica in the following embodiment are treated fillers.
Example 1
Adding 20 parts of silyl-terminated polyether MAX923, 5 parts of silyl-terminated polyether SAX530, 10 parts of diisononyl phthalate, 25 parts of nano active calcium carbonate, 1 part of titanium dioxide, 1 part of antioxidant 1010, 1 part of bis (2, 2, 6, 6-tetramethyl-4-piperidyl) sebacate and 1 part of 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole into a double-planet stirring kettle in sequence, stirring and dispersing at 100-110 ℃ and dehydrating in vacuum for 2 hours, wherein the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding 1 part of vinyl trimethoxy silane into the double-planet stirring kettle, mixing for 30 minutes in vacuum, adding 1.0 part of N-beta-aminoethyl-gamma-aminopropyl trimethoxy silane into the double-planet stirring kettle, mixing for 10 minutes under vacuum state, finally adding 0.5 part of U-220H into a stirring kettle, mixing for 10 minutes under vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is 2Sealing and packaging.
Example 2
Adding 35 parts of silyl-terminated polyether MAX951, 10 parts of silyl-terminated polyether SAX530, 20 parts of diisodecyl phthalate, 25 parts of nano active calcium carbonate, 20 parts of silica powder, 10 parts of titanium dioxide, 2 parts of antioxidant 1076, 2 parts of bis (2, 2, 6, 6-tetramethyl-4-piperidyl) sebacate and 2 parts of 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole into a double-planetary stirring kettle in sequence, stirring and dispersing at 100-110 ℃ and carrying out vacuum dehydration for 2 hours until the vacuum degree is not less than-0.098 MPa, cooling to below 45 ℃, adding 5 parts of vinyltrimethoxysilane into the double-planetary stirring kettle, mixing for 30 minutes under a vacuum state, then adding 5 parts of aminopropyltriethoxysilane into the double-planetary stirring kettle, mixing for 10 minutes under a vacuum state, finally, adding 1 part of U-303 and 1 part of stannous octoate into a stirring kettle, and mixing for 10 minutes in a vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is2Sealing and packaging.
Example 3
30 portions of silyl terminated polyether MAX620, 5 portions of silyl terminated polyether SAX530, 15 portions of SAT010, 25 portions of nano active calcium carbonate, 10 portions of silicon micropowder, 5 portions of carbon black, 1.5 portions of antioxidant 1010, 1.5 portions of bis (2, 2, 6, 6-tetramethyl- 4-piperidyl) sebacate, 1.5 parts of 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole are sequentially added into a double-planet stirring kettle, stirred and dispersed at 100-110 ℃ and vacuum-dehydrated for 2 hours, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to below 45 ℃, 2 parts of vinyltrimethoxysilane is added into the double-planet stirring kettle, the mixture is mixed for 30 minutes under the vacuum state, then 2.5 parts of aminopropyltrimethoxysilane is added into the double-planet stirring kettle, the mixture is mixed for 10 minutes under the vacuum state, finally 1 part of stannous octoate is added into the stirring kettle, the mixture is mixed for 10 minutes under the vacuum state, the vacuum degree is not less than-0.098 MPa, N is2Sealing and packaging.
Example 4
20 parts of silyl-terminated polyether MAX951, 20 parts of silyl-terminated polyether SAX530, 20 parts of diisodecyl phthalate, 15 parts of nano active calcium carbonate, 20 parts of silica powder, 5 parts of fumed silica, 10 parts of titanium dioxide, 1.5 parts of antioxidant 1076, 2 parts of bis (2, 2, 6, 6-tetramethyl-4-piperidyl) sebacate and 2 parts of 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole are sequentially added into a double-planetary stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to the temperature of below 45 ℃, 2.5 parts of vinyl trimethoxy silane is added into the double-planetary stirring kettle, the mixture is mixed for 30 minutes in the vacuum state, and then 1.5 parts of N-beta-aminoethyl-gamma-aminopropyltrimethoxy silane and 1 part of aminopropyltriethoxy silane are added into the double-planetary stirring kettle Mixing in a star stirring kettle for 10 minutes in a vacuum state, finally adding 1.5 parts of U-220H into the stirring kettle, mixing for 10 minutes in the vacuum state, wherein the vacuum degree is not less than-0.098 MPa, and N is 2Sealing and packaging.
The performance comparison tests of the examples 1 to 4 and the general-purpose silyl-terminated polyether sealant are carried out, the mechanical property data are obtained by testing after the sealant is cured for 7 days under the conditions of 23 +/-2 ℃ and 50 +/-5% of relative humidity, and the specific test results are shown in the following table 1.
Test examples
The performance of a silane-terminated sealant of the present invention having excellent media resistance was tested by the following test.
Test example 1
The shear strength was tested according to GB/T7124-2008.
Test example 2
Adhesion: torn by hand.
Test example 3
Rate of change in weight: and weighing the weight of the film before and after soaking.
The general-purpose silane-terminated polyether sealant and the examples 1, 2, 3 and 4 are subjected to performance comparison tests,
very good o: good Δ: general x: difference (D)
The test results in the table show that the silyl-terminated polyether sealant with excellent medium resistance prepared by the invention has good adhesion to various substrates, especially has very good adhesion after soaking in engine oil, and is obviously superior to the domestic common silyl-terminated polyether sealant products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (1)
1. A preparation method of a silane-terminated sealant with excellent medium resistance is characterized by comprising the following steps: (1) adding nano active calcium carbonate into a stirring kettle, heating while stirring, adding a coupling agent gamma-glycidyl ether oxy propyl trimethoxy silane when the temperature is raised to 150 ℃, wherein the dosage of the coupling agent gamma-glycidyl ether oxy propyl trimethoxy silane is 0.3 percent of the total amount of the filler, the dosage of the coupling agent gamma- (methacryloyloxy) propyl trimethoxy silane is 0.6 percent of the total amount of the filler, keeping the temperature at 150 ℃, vacuumizing for 3 hours, closing heating, maintaining the pressure, naturally cooling or cooling by circulating water, and discharging for later use;
(2) 20 parts of terminal silyl polyether MAX923 of KANEKA, 5 parts of terminal silyl polyether SAX530 of KANEKA, 10 parts of diisononyl phthalate,25 parts of the treated nano active calcium carbonate in the step (1), 1 part of titanium dioxide, 1 part of an antioxidant 1010, 1 part of bis (2, 2, 6, 6-tetramethyl-4-piperidyl) sebacate and 1 part of 2- (2 ' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole are sequentially added into a double-planet stirring kettle, stirred, dispersed and vacuum-dehydrated for 2 hours at the temperature of 100-110 ℃, the vacuum degree is not less than-0.098 MPa, the mixture is cooled to below 45 ℃, 1 part of vinyl trimethoxy silane is added into the double-planet stirring kettle and mixed for 30 minutes under the vacuum state, then 1.0 part of N-beta-aminoethyl-gamma-aminopropyl trimethoxy silane is added into the double-planet stirring kettle and mixed for 10 minutes under the vacuum state, finally, 0.5 part of U-220H is added into the stirred tank and mixed for 10 minutes in a vacuum state, the vacuum degree is not less than-0.098 MPa, and N is 2Sealing and packaging.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811233112.6A CN109337631B (en) | 2018-10-23 | 2018-10-23 | Preparation method of silane-terminated sealant with excellent medium resistance |
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| CN201811233112.6A CN109337631B (en) | 2018-10-23 | 2018-10-23 | Preparation method of silane-terminated sealant with excellent medium resistance |
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| CN109337631A CN109337631A (en) | 2019-02-15 |
| CN109337631B true CN109337631B (en) | 2021-02-09 |
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| CN110607074B (en) * | 2019-09-18 | 2021-11-09 | 烟台德邦科技股份有限公司 | UV/moisture dual-curing organic silicon resin composition with excellent weather resistance and preparation method thereof |
| CN115895557A (en) * | 2022-12-19 | 2023-04-04 | 烟台德邦科技股份有限公司 | Preparation of sealant with excellent bonding performance |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004155799A (en) * | 2001-09-27 | 2004-06-03 | Sekisui Chem Co Ltd | Curable composition, sealing material and adhesive |
| CN103602304A (en) * | 2013-11-11 | 2014-02-26 | 苏州毫邦新材料有限公司 | Fast moisture-cured composition |
| CN104479608A (en) * | 2014-12-30 | 2015-04-01 | 北京天山新材料技术有限公司 | Environment-friendly mildewproof silicone-modified polyether sealant |
| CN105176470A (en) * | 2015-09-23 | 2015-12-23 | 烟台德邦科技有限公司 | Silyl-terminated polyether sealant and preparing method thereof |
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2018
- 2018-10-23 CN CN201811233112.6A patent/CN109337631B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004155799A (en) * | 2001-09-27 | 2004-06-03 | Sekisui Chem Co Ltd | Curable composition, sealing material and adhesive |
| CN103602304A (en) * | 2013-11-11 | 2014-02-26 | 苏州毫邦新材料有限公司 | Fast moisture-cured composition |
| CN104479608A (en) * | 2014-12-30 | 2015-04-01 | 北京天山新材料技术有限公司 | Environment-friendly mildewproof silicone-modified polyether sealant |
| CN105176470A (en) * | 2015-09-23 | 2015-12-23 | 烟台德邦科技有限公司 | Silyl-terminated polyether sealant and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 硅烷偶联剂应用技术;苏威;《河北化工》;19901231(第3期);第40-42页 * |
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