CN109337631A - A kind of preparation method for the end-silicane-group sealant that resistance to medium is excellent - Google Patents
A kind of preparation method for the end-silicane-group sealant that resistance to medium is excellent Download PDFInfo
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- CN109337631A CN109337631A CN201811233112.6A CN201811233112A CN109337631A CN 109337631 A CN109337631 A CN 109337631A CN 201811233112 A CN201811233112 A CN 201811233112A CN 109337631 A CN109337631 A CN 109337631A
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- stirred tank
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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
-
- 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
- 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
-
- 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 present invention relates to a kind of preparation methods of end-silicane-group sealant that resistance to medium is excellent, it include: by silyl-terminated polyether, plasticizer, pretreated filler, pigment, antioxidant, UV absorbers, light stabilizer sequentially adds in double-planet stirred tank, it is dispersed with stirring under the conditions of 100~110 DEG C simultaneously vacuum dehydration 2 hours, vacuum degree is not less than -0.098MPa, it is cooled to 45 DEG C or less, deicer is added in double-planet stirred tank, it mixes 30 minutes under vacuum conditions, then by tackifier, catalyst is added in stirred tank, it mixes 10 minutes under vacuum conditions, N2Preservation and packaging.A kind of excellent end-silicane-group sealant of resistance to medium provided by the invention, single-component package is easy to be glued, and cured glue layer is to a variety of substrates bonding force with higher, adhesive strength conservation rate is high after machine oil impregnates, and can meet the safe handling of the industries such as automobile, locomotive very well.
Description
Technical field
The present invention relates to a kind of preparation method of end-silicane-group sealant that resistance to medium is excellent more particularly to a kind of resistance to machines
The preparation method of the strong silane modified polyether seal glue of oil, bonding force.
Background technique
It is close that silyl-terminated polyether type elastic sealant is also known as organosilicon modified polyether sealant, modified silicone seal gum and MS
Sealing.It has extensive application originating from Japan in building trade.The country is introduced in recent years, is slowly familiar with by compatriots, due to
It has the characteristics that paintability, it is good to most of substrate bonding power, without solvent, have more applications within nearly 1 year,
Some occasions can partially substitute silicone sealant or polyurethane adhesive, be applied to the fields such as automobile, locomotive.
Summary of the invention
The present invention provides a kind of preparation method of end-silicane-group sealant that resistance to medium is excellent, sealing prepared by the present invention
Glue has resistance to machine oil function admirable, has good cementability on most of substrates, can be good at meeting product and used
Reliability requirement in journey.
A kind of preparation method of the excellent end-silicane-group sealant of resistance to medium of the present invention, comprising:
(1) pretreatment of filler: filler being added in stirred tank, is heated while stirring, and when being warming up to 150 DEG C, coupling agent is added
γ-glycidyl ether oxypropyltrimethoxysilane KH560, dosage are the 0.3% and coupling agent A174 [γ-of filler total amount
(methacryloxypropyl) propyl trimethoxy silicane], dosage is the 0.6% of filler total amount, kept for 150 DEG C, after vacuumizing 3 hours,
Pass is heated, pressure maintaining, is discharged after natural cooling or circulating water cooling spare；
(2) by 25~45 parts of silyl-terminated polyethers, 10~20 parts of plasticizer, the filler of 25~45 parts of steps (1), 1~10 part of face
Material, 1~2 part of antioxidant, 1~2 part of UV absorbers, 1~2 part of light stabilizer sequentially add in double-planet stirred tank, 100
It is dispersed with stirring under the conditions of~110 DEG C simultaneously vacuum dehydration 2 hours, vacuum degree is not less than -0.098MPa, is cooled to 45 DEG C hereinafter, will
1~5 part of deicer is added in double-planet stirred tank, mixes 30 minutes, 1~5 part of tackifier is added under vacuum conditions then
In stirred tank, mixes 10 minutes, finally 0.5~2 part of catalyst is added in stirred tank, under vacuum conditions under vacuum conditions
Mixing 10 minutes, vacuum degree are not less than -0.098MPa, N2Preservation and packaging.
The resistance to medium and resistance to settling of filler are increased to the pretreatment of filler, based on the above technical solution,
The present invention can also be improved as follows.
Further, the silyl-terminated polyether is in MAX923, MAX951, MAX602, SAX530 of Japan KANEKA
One or more of mixtures.
Beneficial effect using these types of silyl-terminated polyether is: they are all acrylic acid modified silyl-terminated polyethers,
After introducing acrylic acid in segment, the polarity of polymer is increased, the resistance to machine oil performance of sealant is improved.
Further, the plasticizer be diisononyl phthalate (DINP), diisooctyl phthalate (DIDP),
The SAT010 of Japanese KANEKA.
Further, the filler is the mixed of one or more of nm-class active calcium carbonate, silicon powder, fumed silica
Close object.
Further, the pigment is one of titanium dioxide, carbon black.
Further, the antioxidant is one of antioxidant 1010 and antioxidant 1076.
Further, the light stabilizer is bis- (2,2,6,6--4-piperidyl of tetramethyl) sebacates.
Further, the UV absorbers are that 2- (2 '-hydroxyls -3 '-tertiary butyl -5 '-aminomethyl phenyl) -5- chlorobenzene is simultaneously
Triazole.
Further, the deicer is vinyltrimethoxysilane.
Further, the tackifier are N- β-aminoethyl-γ-aminopropyltrimethoxysilane, aminopropyl trimethoxy silicon
The mixture of one or more of alkane, aminopropyl triethoxysilane.
Further, the catalyst is the mixed of one or more of U-220H, U-303 of day east chemical conversion, stannous octoate
Close object.
The beneficial effects of the present invention are: the end-silicane-group sealant that a kind of resistance to medium provided by the invention is excellent, single group
Subpackage dress, is easy to be glued, and cured glue layer is to a variety of substrates bonding force with higher, adhesive strength conservation rate after machine oil impregnates
Height can meet the safe handling of the industries such as automobile, locomotive very well.
Specific embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
The pretreatment of filler: filler being added in stirred tank, is heated while stirring, and when being warming up to 150 DEG C, coupling agent is added
KH560 (γ-glycidyl ether oxypropyltrimethoxysilane), dosage are the 0.3% and coupling agent A174 [γ-of filler total amount
(methacryloxypropyl) propyl trimethoxy silicane], dosage is the 0.6% of filler total amount, kept for 150 DEG C, after vacuumizing 3 hours,
Close heating, pressure maintaining discharges after natural cooling or circulating water cooling spare, nm-class active calcium carbonate in following embodiment, silicon powder,
Fumed silica is processed filler.
Embodiment 1
By 20 parts of silyl-terminated polyether MAX923,5 parts of silyl-terminated polyether SAX530,10 parts of diisononyl phthalates, 25
Part nm-class active calcium carbonate, 1 part of titanium dioxide, 1 part of antioxidant 1010,1 part of bis- (2,2,6,6--4-piperidines of tetramethyl
Base) sebacate, 1 part of 2- (2 '-hydroxyls -3 '-tertiary butyl -5 '-aminomethyl phenyl) -5- chlorobenzotriazole sequentially adds double-planet
In stirred tank, it is dispersed with stirring under the conditions of 100~110 DEG C simultaneously vacuum dehydration 2 hours, vacuum degree is not less than -0.098MPa, cold
But to 45 DEG C hereinafter, 1 part of vinyltrimethoxysilane is added in double-planet stirred tank, 30 points of mixing under vacuum conditions
Clock 1.0 parts of N- β-aminoethyl-γ-aminopropyltrimethoxysilanes is added in double-planet stirred tank later, under vacuum conditions
0.5 part of U-220H is finally added in stirred tank and mix under vacuum conditions 10 minutes by mixing 10 minutes, vacuum degree not less than-
0.098MPa , N2Preservation and packaging.
Embodiment 2
By 35 parts of silyl-terminated polyether MAX951,10 parts of silyl-terminated polyether SAX530,20 parts of diisooctyl phthalates, 25
Part nm-class active calcium carbonate, 20 parts of silicon powders, 10 parts of titanium dioxides, 2 parts of antioxidant 1076s, 2 parts of bis- (2,2,6,6- tetramethyls
Base-4-piperidyl) sebacate, 2 parts of 2- (2 '-hydroxyls-3 '-tertiary butyl-5 '-aminomethyl phenyl)-5- chlorobenzotriazoles according to
In secondary addition double-planet stirred tank, be dispersed with stirring under the conditions of 100~110 DEG C and vacuum dehydration 2 hours, vacuum degree not less than-
0.098MPa is cooled to 45 DEG C hereinafter, 5 parts of vinyltrimethoxysilanes are added in double-planet stirred tank, in vacuum shape
It is mixed under state 30 minutes, 5 parts of aminopropyl triethoxysilanes is added in double-planet stirred tank later, mix under vacuum conditions
10 minutes, finally 1 part of U-303 and 1 part of stannous octoate is added in stirred tank, is mixed 10 minutes under vacuum conditions, vacuum degree
Not less than -0.098MPa, N2Preservation and packaging.
Embodiment 3
By 30 parts of silyl-terminated polyether MAX620,5 parts of silyl-terminated polyether SAX530,15 parts of SAT010,25 parts of nano active carbons
Sour calcium, 10 parts of silicon powders, 5 parts of carbon blacks, 1.5 parts of antioxidant 1010s, 1.5 parts of bis- (2,2,6,6--4-piperidines of tetramethyl
Base) sebacate, 1.5 parts of 2- (2 '-hydroxyls -3 '-tertiary butyl -5 '-aminomethyl phenyl) -5- chlorobenzotriazoles sequentially add duplicate rows
In star stirred tank, it is dispersed with stirring under the conditions of 100~110 DEG C simultaneously vacuum dehydration 2 hours, vacuum degree is not less than -0.098MPa,
45 DEG C are cooled to hereinafter, 2 parts of vinyltrimethoxysilanes are added in double-planet stirred tank, 30 points of mixing under vacuum conditions
2.5 parts of aminopropyl trimethoxysilanes are added in double-planet stirred tank later for clock, under vacuum conditions mixing 10 minutes, most
1 part of stannous octoate is added in stirred tank afterwards, is mixed 10 minutes under vacuum conditions, vacuum degree is not less than -0.098MPa, N2
Preservation and packaging.
Embodiment 4
By 20 parts of silyl-terminated polyether MAX951,20 parts of silyl-terminated polyether SAX530,20 parts of diisooctyl phthalates, 15
Part nm-class active calcium carbonate, 20 parts of silicon powders, 5 parts of fumed silicas, 10 parts of titanium dioxides, 1.5 parts of antioxidant 1076s, 2 parts double
(2,2,6,6--4-piperidyl of tetramethyl) sebacate, 2 parts of 2- (2 '-hydroxyls-3 '-tertiary butyl-5 '-methylbenzene
Base) -5- chlorobenzotriazole sequentially adds in double-planet stirred tank, it is dispersed with stirring under the conditions of 100~110 DEG C and vacuum dehydration 2
Hour, vacuum degree is not less than -0.098MPa, is cooled to 45 DEG C hereinafter, duplicate rows is added in 2.5 parts of vinyltrimethoxysilanes
In star stirred tank, mix 30 minutes under vacuum conditions, later by 1.5 parts of N- β-aminoethyl-γ-aminopropyltrimethoxysilanes
It is added in double-planet stirred tank, mixes 10 minutes under vacuum conditions, finally by 1.5 parts with 1 part of aminopropyl triethoxysilane
U-220H is added in stirred tank, mixes 10 minutes under vacuum conditions, and vacuum degree is not less than -0.098MPa, N2Preservation and packaging
?.
Embodiment 1 to 4 and universal silyl-terminated polyether sealant are done into performance comparison test, mechanical performance data exists
23 ± 2 DEG C, gained is tested after solidifying 7 days under conditions of relative humidity 50 ± 5%, specific test result see the table below 1.
Test example
Pass through a kind of performance of the excellent end-silicane-group sealant of following experimental test resistance to medium of the invention.
Test example 1
Shear strength is tested according to GB/T 7124-2008.
Test example 2
Cementability: it is pulled with tearing.
Test example 3
Weight rate: the weight that film impregnates front and back is weighed.
Universal silyl-terminated polyether sealant and embodiment 1,2,3,4 are subjected to performance contrast test,
◎: very zero: good △: general ×: it is poor
It can be seen that a kind of excellent silyl-terminated polyether sealant of resistance to medium prepared by the present invention from the test result of upper table,
Good to a variety of substrate bondings, bonding force is still very good after immersion test especially in machine oil, hence it is evident that common better than domestic
Silyl-terminated polyether sealant product.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of preparation method for the end-silicane-group sealant that resistance to medium is excellent characterized by comprising
(1) pretreatment of filler: filler being added in stirred tank, is heated while stirring, and when being warming up to 150 DEG C, coupling agent is added
γ-glycidyl ether oxypropyltrimethoxysilane KH560, dosage are 0.3% and coupling agent γ-(methyl-prop of filler total amount
Alkene acyl-oxygen) propyl trimethoxy silicane A174, dosage is the 0.6% of filler total amount, is kept for 150 DEG C, after vacuumizing 3 hours, Guan Jia
It discharges after heat, pressure maintaining, natural cooling or circulating water cooling spare；
(2) by 25~45 parts of silyl-terminated polyethers, 10~20 parts of plasticizer, the filler of 25~45 parts of steps (1), 1~10 part of face
Material, 1~2 part of antioxidant, 1~2 part of UV absorbers, 1~2 part of light stabilizer sequentially add in double-planet stirred tank, 100
It is dispersed with stirring under the conditions of~110 DEG C simultaneously vacuum dehydration 2 hours, vacuum degree is not less than -0.098MPa, is cooled to 45 DEG C hereinafter, will
1~5 part of deicer is added in double-planet stirred tank, mixes 30 minutes, 1~5 part of tackifier is added under vacuum conditions then
In stirred tank, mixes 10 minutes, finally 0.5~2 part of catalyst is added in stirred tank, under vacuum conditions under vacuum conditions
Mixing 10 minutes, vacuum degree are not less than -0.098MPa, N2Preservation and packaging.
2. preparation method according to claim 1, which is characterized in that the silyl-terminated polyether is Japan KANEKA's
The mixture of one or more of MAX923, MAX951, MAX602, SAX530.
3. preparation method according to claim 1, which is characterized in that the plasticizer be diisononyl phthalate,
One of diisooctyl phthalate, SAT010 of Japan KANEKA；The filler is nm-class active calcium carbonate, silicon is micro-
The mixture of one or more of powder, fumed silica；The pigment is one of titanium dioxide, carbon black；The antioxygen
Agent is one of antioxidant 1010 and antioxidant 1076；The light stabilizer is bis- (2,2,6,6- tetramethyls-4-
Piperidyl) sebacate；The UV absorbers are 2- (2 '-hydroxyls -3 '-tertiary butyl -5 '-aminomethyl phenyl) -5- chlorobenzene
And triazole；The deicer is vinyltrimethoxysilane；The tackifier are N- β-aminoethyl-γ-aminopropyl trimethoxy
Base silane, γ-methacryloxypropyl trimethoxy silane, aminopropyl trimethoxysilane, aminopropyl-triethoxy silicon
The mixture of one or more of alkane；The catalyst is one of U-220H, U-303 of day east chemical conversion, stannous octoate
Or several mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811233112.6A CN109337631B (en) | 2018-10-23 | 2018-10-23 | Preparation method of silane-terminated sealant with excellent medium resistance |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 true CN109337631A (en) | 2019-02-15 |
| CN109337631B CN109337631B (en) | 2021-02-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607074A (en) * | 2019-09-18 | 2019-12-24 | 烟台德邦科技有限公司 | 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 |
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|---|---|---|---|---|
| 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 |
-
2018
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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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110607074A (en) * | 2019-09-18 | 2019-12-24 | 烟台德邦科技有限公司 | UV/moisture dual-curing organic silicon resin composition with excellent weather resistance and preparation method thereof |
| 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 |
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| CN109337631B (en) | 2021-02-09 |
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