CN109679556A - Preparation method of environment-friendly silane modified sealant - Google Patents
Preparation method of environment-friendly silane modified sealant Download PDFInfo
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- CN109679556A CN109679556A CN201811561341.0A CN201811561341A CN109679556A CN 109679556 A CN109679556 A CN 109679556A CN 201811561341 A CN201811561341 A CN 201811561341A CN 109679556 A CN109679556 A CN 109679556A
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- silane
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- 239000000565 sealant Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 title abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- 239000004611 light stabiliser Substances 0.000 claims abstract description 11
- 239000003707 silyl modified polymer Substances 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 5
- 239000000049 pigment Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- -1 methoxyl group Chemical group 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 7
- 239000003292 glue Substances 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 239000012974 tin catalyst Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 235000010216 calcium carbonate Nutrition 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229920000647 polyepoxide Chemical class 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 2
- 235000019241 carbon black Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000004526 silane-modified polyether Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid group Chemical group C(CCC(=O)O)(=O)O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical class COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007969 cellular immunity Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 210000004087 cornea Anatomy 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002320 enamel (paints) Chemical class 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 125000003700 epoxy group Chemical class 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 210000004324 lymphatic system Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005553 polystyrene-acrylate Polymers 0.000 description 1
- 229920002635 polyurethane Chemical class 0.000 description 1
- 239000004814 polyurethane Chemical class 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- NQRYJNQNLNOLGT-UHFFFAOYSA-N tetrahydropyridine hydrochloride Natural products C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 1
- 210000001541 thymus gland Anatomy 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 210000004885 white matter Anatomy 0.000 description 1
Classifications
-
- 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
- C09J171/02—Polyalkylene oxides
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a preparation method of an environment-friendly silane modified sealant, which comprises the following steps: sequentially adding 30-50 parts of silane-terminated polymer, 10-20 parts of plasticizer, 5-40 parts of filler, 0-10 parts of pigment, 1-2 parts of light stabilizer and 1-2 parts of antioxidant into a stirring kettle, stirring and dispersing at 100-110 ℃, performing vacuum dehydration for 2 hours, cooling to below 45 ℃, adding 1-5 parts of water removing agent into the stirring kettle, adding 1-5 parts of tackifier into the stirring kettle, adding 2-4 parts of catalyst into the stirring kettle, mixing for 15 minutes, and adding N2Sealing and packaging; the environment-friendly sealant provided by the invention does not contain organic tin catalysts and o-benzene plasticizers, meets European Union export standards, can pass the authentication of ROHS, REACH and the like, is packaged in single components, is easy to glue, can be cured quickly, has good adhesive force on various substrates, and has excellent aging resistance.
Description
Technical field
The present invention relates to a kind of preparation method of the silane-modified sealant of environment-friendly type more particularly to a kind of rapid curing, no
The preparation method of environment-friendly type silane modified polyether seal glue containing organotin catalysts, belongs to adhesive field.
Background technique
Japan is the country for developing silane-modified sealant product earliest, and enters market the eighties in last century,
Since its polymer is low with viscosity, storage stability is very good, can have good Binder Phase with most substrates without primary coat
Many advantages, such as capacitive, good surface paintability, purposes is more and more extensive.It is improved by continuing to optimize, bonding range is
Engineering plastics (such as PVC, ABS, polystyrene and polyacrylate are expanded to from pore-free material (such as glass, metal substrate)
Deng), various lacquer paintings (such as esters of acrylic acid, epoxies, polyurethanes and enamel paint class paint are expanded to from general substrate surface
Face), bonding range is wide, to the adaptability of substrate strong, has had reached the height that other similar products are difficult to reach.
Since silane modified polyether polymer reaction activity is lower, it can just be made by needing to be added a large amount of organotin catalysts
Solidification, and organotin catalysts are harmful, major determinant to organism are as follows: central nervous system will cause white matter of brain water
Swollen, thymus gland and the inhibiting effect of lymphatic system, cellular immunity are harmed, hormone secretion inhibition causes diabetes and high fat of blood
Deng；To the toxicity of people: part is to skin, respiratory tract, stimulation of cornea etc..Environmental protection consciousness and health perception increasingly
Today of raising, requiring the environmental issue of adhesive will be further stringent, protect environment and health of human body to seem even more important, especially
It is that European Union's aspect has done stringent limitation or disabling to the use of organotin catalysts in product, and this requires us must
The solidification that can substitute the substances of organotin catalysts to promote silane-modified sealant must be found as early as possible.
Summary of the invention
Technical scheme is as follows: the system of a kind of rapid curing, environment-friendly type sealant without organotin catalysts
Preparation Method includes: by 30~50 parts of silane-terminated polymers, 10~20 parts of plasticizer, 5~40 parts of fillers, 0~10 part of pigment, 1
~2 parts of light stabilizers, 1~2 part of antioxidant sequentially add in double-planet stirred tank, are dispersed with stirring simultaneously under the conditions of 100~110 DEG C
Vacuum dehydration 2 hours, vacuum degree was not less than -0.098MPa, is cooled to 45 DEG C and stirs hereinafter, double-planet is added in 1~5 part of deicer
It mixes in kettle, mixes under vacuum conditions 30 minutes, then 1~5 part of tackifier is added in stirred tank, mixes under vacuum conditions
15 minutes, finally 2~4 parts of catalyst are added in stirred tanks, are mixed 15 minutes under vacuum conditions, vacuum degree not less than-
0.098MPa,N2Preservation and packaging.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the silane-terminated polymer is the polymer for having the following structure formula (1) or structural formula (2):
R1=methyl, ethyl, methoxyl group, ethyoxyl
R2=methoxyl group, ethyoxyl
R3=-CH2-、-(CH2)3-
Further, the plasticizer is polypropylene glycol (PPG-400, PPG-2000, PPG-3000 etc.).
Further, the filler is nanometer calcium carbonate, aluminium oxide, aluminium hydroxide, one in hydrophobic type gas phase silica
Kind or several mixtures.
Further, the pigment is one of titanium dioxide, carbon black.
Further, the light stabilizer is succinic acid and (4- hydroxyl -2,2, the polymerization of 6,6- tetramethyl -1- piperidine alcohols
Object), i.e. light stabilizer 622.
Further, the antioxidant is antioxidant B215.
Further, the deicer is vinyltrimethoxysilane.
Further, the tackifier are aminopropyl trimethoxysilane and γ-(2,3- the third oxygen of epoxy) propyl trimethoxy
The mixture of silane, mixed proportion: mass ratio 1:0.5~1:1.
Further, it (includes: KRBi-3, KRBi-5, De Yin of the triumphant auspicious chemistry in Changzhou that the catalyst, which is organic bismuth catalyst,
DY-20, the MB-20 of U.S.'s gas companies etc. of chemistry) and 2 ethyl hexanoic acid and 2,3,4,6,7,8,9,10- octahydro pyrimido
The mixture of the compound (1:1) of [1,2-a] azatropylidene.
The beneficial effects of the present invention are: a kind of environment-friendly type sealant provided by the invention, is free of organotin catalysts and neighbour
Benzene class plasticizer, meets European Union's export standard, can be authenticated by ROHS, REACH etc., and single-component package is easy to be glued, can be fast
Speed solidification has good bonding force to a variety of substrates, and ageing-resistant performance is excellent.
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.
Embodiment 1
By 30 parts of silane-terminated polymers, structural formula is
10 parts of polypropylene glycols, 5 parts of hydrophobic type gas phase silicas, 1 part of light stabilizer, 622,1 part of antioxidant B215 successively add
Enter in 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, 1 part of vinyltrimethoxysilane is added in double-planet stirred tank, in vacuum state
Lower mixing 30 minutes, later by 0.5 part of aminopropyl trimethoxysilane and 0.5 part of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy
Base silane is added in double-planet stirred tank, mixes 15 minutes under vacuum conditions, finally by 1 part of organic bismuth catalyst KRBi-3,1
Stirred tank is added in the compound (1:1) of part 2 ethyl hexanoic acid and 2,3,4,6,7,8,9,10- octahydro pyrimido [1,2-a] azatropylidene
It is interior, it mixes 15 minutes under vacuum conditions, vacuum degree is not less than -0.098MPa, N2Preservation and packaging.
Embodiment 2
By 50 parts of silane-terminated polymers, structural formula is
20 parts of polypropylene glycols, 20 parts of nanometer calcium carbonates, 20 parts of aluminium oxide, 10 parts of titanium dioxides, 2 parts 622,2 parts of light stabilizer
Antioxidant B215 is sequentially added in double-planet stirred tank, is dispersed with stirring under the conditions of 100~110 DEG C and vacuum dehydration 2 hours, very
Reciprocal of duty cycle is not less than -0.098MPa, is cooled to 45 DEG C hereinafter, 5 parts of vinyltrimethoxysilanes are added in double-planet stirred tanks,
It mixes 30 minutes under vacuum conditions, later by 2 parts of aminopropyl trimethoxysilanes and 2 parts of γ-(2,3- the third oxygen of epoxy) propyl
Trimethoxy silane is added in double-planet stirred tank, mixes 15 minutes under vacuum conditions, finally by 2 parts of organic bismuth catalysts
The compound (1:1) of KRBi-5,2 parts of 2 ethyl hexanoic acids and 2,3,4,6,7,8,9,10- octahydro pyrimido [1,2-a] azatropylidenes add
Enter in stirred tank, mix 15 minutes under vacuum conditions, vacuum degree is not less than -0.098MPa, N2Preservation and packaging.
Embodiment 3
By 40 parts of silane-terminated polymers, structural formula is
15 parts of polypropylene glycols, 20 parts of nanometer calcium carbonates, 20 parts of aluminium hydroxides, 5 parts of carbon blacks, 1.5 parts of light stabilizers 622,1.5
Part antioxidant B215 is sequentially added in double-planet stirred tank, 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, is cooled to 45 DEG C hereinafter, double-planet stirred tank is added in 3 parts of vinyltrimethoxysilanes
It is interior, it mixes 30 minutes under vacuum conditions, later by 1.5 parts of aminopropyl trimethoxysilanes and 1.5 parts of γ-(2,3- epoxies third
Oxygen) propyl trimethoxy silicane be added double-planet stirred tank in, under vacuum conditions mix 15 minutes, it is finally organic by 1.5 parts
Bismuth catalyst DY-20,1.5 parts of 2 ethyl hexanoic acids and 2, the chemical combination of 3,4,6,7,8,9,10- octahydro pyrimido [1,2-a] azatropylidenes
Object (1:1) is added in stirred tank, mixes 15 minutes under vacuum conditions, and vacuum degree is not less than -0.098MPa, N2Preservation and packaging is
It can.
Embodiment 4
By 40 parts of silane-terminated polymers, structural formula is
15 parts of polypropylene glycols, 5 parts of hydrophobic type gas phase silicas, 25 parts of aluminium hydroxides, 1.5 parts of light stabilizers 622,1.5
Part antioxidant B215 is sequentially added in double-planet stirred tank, 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, is cooled to 45 DEG C hereinafter, double-planet stirring is added in 2.5 parts of vinyltrimethoxysilanes
In kettle, mix 30 minutes under vacuum conditions, later by 2 parts of aminopropyl trimethoxysilanes and 1.0 parts of γ-(2,3- epoxies third
Oxygen) propyl trimethoxy silicane be added double-planet stirred tank in, under vacuum conditions mix 15 minutes, it is finally organic by 1.0 parts
Bismuth catalyst MB-20,2 parts of 2 ethyl hexanoic acids and 2, the compound of 3,4,6,7,8,9,10- octahydro pyrimido [1,2-a] azatropylidenes
(1:1) is added in stirred tank, mixes 15 minutes under vacuum conditions, and vacuum degree is not less than -0.098MPa, N2Preservation and packaging is
It can.
Embodiment 1 to 4 and the silane-modified sealant of tin catalytic type are done into performance comparison test, mechanical performance data is 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
Organotin catalysts, rapid curing, to substrate adhesive force are free of by following experimental test one kind of the invention
It is good, the performance of the excellent Environment-friendlyadhesive adhesive of aged properties.
Test example 1
Surface drying time: it is tested according to GB/T13477.5-2002.
Test example 2
Extrusion rate: pressure 0.6MPa, glue discharging mouth φ 3
Test example 3
Curing depth: 25 DEG C, cured thickness for 24 hours under 50% relative humidities
Test example 4
Adhesive strength: it is tested according to GB/T 7124-2008.
The universal silane-modified sealant containing tin catalyst and embodiment 1,2,3,4 are subjected to performance contrast test,
Test result see the table below.
It can be seen that this environment-friendly type silane without organotin catalysts prepared by the present invention from the test result of upper table
Modified sealant, compared with organotin catalyzed silane-modified sealant, surface drying time, extrusion rate, curing depth, storage are stablized
Property, adhesive strength, resistance to ag(e)ing etc. are almost the same, can substitute completely existing containing the silane-modified of organotin catalysts
Sealant, can meet very well client for silane-modified sealant performance and environmental protection high standards, meet RoHS and
The strict demand of REACH.
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 of the silane-modified sealant of environment-friendly type characterized by comprising Silante terminated poly- by 30~50 parts
Object, 10~20 parts of plasticizer, 5~40 parts of fillers, 0~10 part of pigment, 1~2 part of light stabilizer, 1~2 part of antioxidant is closed successively to add
Enter in 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, mixing 30 under vacuum conditions in 1~5 part of deicer addition double-planet stirred tank
Minute, then 1~5 part of tackifier is added in stirred tank, is mixed 15 minutes under vacuum conditions, finally by 2~4 parts of catalyst
It is added in stirred tank, mixes 15 minutes under vacuum conditions, vacuum degree is not less than -0.098MPa, N2Preservation and packaging；
The catalyst is organic bismuth catalyst and 2 ethyl hexanoic acid and 2,3,4,6,7,8,9,10- octahydro pyrimido [1,2-a]
The mixture of the compound quality ratio 1:1 of azatropylidene.
2. preparation method according to claim 1, which is characterized in that the silane-terminated polymer be structural formula (1) or
The polymer of structural formula (2):
Structural formula (1)
Structural formula (2)
Wherein n=50~150,
R1=methyl, ethyl, methoxyl group, ethyoxyl, R2=methoxyl group, ethyoxyl, R3=-CH2-、-(CH2)3-。
3. preparation method according to claim 1, which is characterized in that the plasticizer is polypropylene glycol PPG-400, PPG-
2000, one of PPG-3000, the filler are nanometer calcium carbonate, aluminium oxide, aluminium hydroxide, hydrophobic type gas phase silica
One or more of mixture, the light stabilizer be light stabilizer 622, the antioxidant be antioxidant B215, it is described
Deicer is vinyltrimethoxysilane, and the tackifier are aminopropyl trimethoxysilane and γ-(2,3- the third oxygen of epoxy)
The mixture of propyl trimethoxy silicane, mixed proportion: mass ratio 1:0.5~1:1.
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| CN112680161A (en) * | 2020-12-23 | 2021-04-20 | 东莞市瑞朗电子有限公司 | Curing sealing adhesive and preparation method thereof |
| CN112920770A (en) * | 2021-03-10 | 2021-06-08 | 浙江亚厦装饰股份有限公司 | Adhesive for adhering prefabricated member of assembled ceiling and preparation method thereof |
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| CN113292958A (en) * | 2021-05-20 | 2021-08-24 | 山东沃赛新材料科技有限公司 | High-transparency environment-friendly silane modified polyether sealant and preparation method thereof |
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Address after: No.3-3 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant after: Yantai Debang Technology Co.,Ltd. Address before: No.3-3 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant before: DARBOND TECHNOLOGY Co.,Ltd. |
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Application publication date: 20190426 |