CN107603549A - A kind of high resiliency silane modified polyether seal glue and preparation method thereof - Google Patents
A kind of high resiliency silane modified polyether seal glue and preparation method thereof Download PDFInfo
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- CN107603549A CN107603549A CN201710840690.5A CN201710840690A CN107603549A CN 107603549 A CN107603549 A CN 107603549A CN 201710840690 A CN201710840690 A CN 201710840690A CN 107603549 A CN107603549 A CN 107603549A
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Abstract
The invention discloses a kind of high resiliency silane modified polyether seal glue and preparation method thereof, it is made up of the raw material of following parts by weight：0.05 0.15 parts of 20 35 parts of silane modified polyether resin, 55 parts of nano-calcium carbonate Ca45,1.5 2.5 parts of aerosil, 15 25 parts of plasticizer, 1.5 2.5 parts of deicer, 0.5 1.5 parts of coupling agent, 0.05 0.15 parts of curing agent and catalyst.Fluid sealant prepared by the present invention has excellent water resistance, elastic recovery rate, weather resistance, mechanical property etc., constituent is relatively simple, cost is cheap, preparation technology is simple, power consumption is low, cost is low, is adapted to industrialized production, has good economic benefit and social benefit.
Description
Technical field
The invention belongs to chemical material technical field, specifically a kind of high resiliency silane modified polyether seal glue and its preparation
Method.
Background technology
Fluid sealant, which is generally used for building, road, bridge, runway etc., has the caulking sealing of retractility seam and connection close
Envelope.In building field, special requirement fluid sealant has the characteristics such as low modulus, elastic recovery rate, can effectively absorb and compensate dynamic
State load, uniformly transfers stress, prevents the generation of the bond damage in long-term dynamics Displacement-deformation.Modern society defends to environment
Raw, safety requirement is increasingly strict, and building maximizes, be diversified, high stratification and the fast development of long service life, to sealing for building
The performance of glue proposes requirements at the higher level.Silicone adhesive and polyurethane adhesive are two kinds that present building is most widely used with industrial circle
Fluid sealant.Silicone adhesive has excellent weather resistance, but adhesion strength is relatively low, and residual small molecule is also easy to produce surface contamination, ornamental poor.It is poly-
Urethane fluid sealant adhesion strength is high, and elasticity is good, but the carbon dioxide discharged during solidification easily bubbles, and weather resistance is poor, to aluminium
Silane coupling agent is needed to use with the bonding of the material such as glass, and the isocyanate group to dissociate after solidifying has larger toxicity.
Silane modified polyether seal glue（MS glue）It is a kind of using alkoxysilane-terminated polyether prepolymer as base-material, with filling out
Material（Calcium carbonate etc.）, the sticky paste that is obtained after physics water removal mixing such as plasticizer and auxiliary agent.MS glue is widely used
In fields such as assembled architecture, track traffic, automobile making, container, elevator and interior decorations.MS glue is without formaldehyde and different
Cyanate, solvent-free, nontoxic, tasteless, VOC is discharged well below national standard, is most environmentally friendly fluid sealant product.Silane changes
The advantages of property polyethers glue has silicone sealant and polyurethane sealant concurrently.
The A of patent CN 102994034 disclose a kind of low modulus single component silane modified polyether seal glue and its preparation
Method.The polyethers that the fluid sealant is modified by trimethoxysilyl or methyl dimethoxy epoxide monosilane, phthalate
The thixotropic agent such as the pigment such as plasticizer, titanium dioxide, filler, polyamide wax, ultra-violet absorber, catalyst, dehydrating agent and adhesive force
The modulation of the raw materials such as accelerator forms.In preparation process, filler vacuum dehydration at a temperature of 105 DEG C, it is desirable to which moisture reaches
Less than 5/10000ths.So harsh moisture control, is difficult in actual production process.
The A of patent CN 106634771 disclose a kind of silane modified polyether seal glue and preparation method thereof.The patent institute
It is the PPOX ether that end group is methoxyl group with resin, extending fillers are powdered whiting, nano-calcium carbonate etc., wherein using
Single-ended alkoxysilane group polyethers effectively increases the initial bonding strength of silane modified polyether seal glue, drawn as reactive diluent
Stretch intensity and reach more than 1.5MPa, however as the increase of initial bonding strength, elongation significantly decreases trend, be unfavorable for its
Application in terms of building field.
The A of patent CN 106634768 disclose it is a kind of soak the excellent silane modified polyether seal glue of adhesive property and its
Preparation method.Filler is nano-calcium carbonate of the surface through oleic acid hydrophobic treatment, and particle diameter 70-100nm, silane modified polyether is day
S203H, S303H of this KENAKE companies production, and add the silicon powder that particle diameter is below 8um and the tree that particle diameter is 60-120nm
Lipid microspheres are as additive, and the modulus of gained fluid sealant is low, and average 100% modulus is 0.2, stretch breaking strength average out to 0.5MPa, is put down
Equal elongation 450%.Fluid sealant prepared by this method has preferable adhesive property, but tensile strength is relatively low, and elongation is not high,
Compared with traditional silicone adhesive, the advantage unobvious in terms of mechanical property.
The A of patent CN 104087228 disclose a kind of low modulus end-silicane-group modified polyether seal glue and its preparation side
Method.It is the mixed of nano-calcium carbonate and powdered whiting that the plasticizer, which is molecular weight in 600-5000 PPG, filler,
Compound, silane modified polyether compound are to hold silicone-modified polyether compound, molecular weight 6000-20000.But this method exists
In preparation process, the mode that filler is added portionwise has been used, to reduce the influence of filler moisture, has added the complexity of technique.
Patent CN 104059592A disclose a kind of one-component silane modified polyether seal glue and preparation method thereof.Its by
Raw material including following percentage by weight reacts to obtain：30-50% silane modified polyether performed polymer, 5-20% plasticizer, 2-
5% admire white powder, 30-50% calcium carbonate, 0.5-1.5% coupling agent 1,0.5-1.5% coupling agent 2,0.5-1.5% stabilization
Agent, 0.5-1.5% UV absorbers, 0.1-1.0% catalyst U-220H.This method prepares gained fluid sealant 100% and stretched
Intensity is 0.7-0.9MPa, fracture tensile strength 1.8-2.0MPa, and the modulus of fluid sealant is higher, does not meet adhesive for building modulus
≤ 0.4MPa requirement.
Silane-modified fluid sealant prepared by prior art can't meet the requirement of low modulus, elastic recovery rate simultaneously,
Therefore, it is necessary to provide high low modulus one-component silane modified polyether seal glue of a kind of elastic recovery rate and preparation method thereof.
The content of the invention
The problem of present invention exists for existing fluid sealant, there is provided a kind of low modulus, high resiliency one-component are silane-modified poly-
Ether fluid sealant and preparation method thereof.
In order to realize the above object the technical solution adopted by the present invention is as follows：
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Silane modified polyether resin 20-
35 parts, nano-calcium carbonate 45-55 parts, aerosil 1.5-2.5 parts, plasticizer 15-25 parts, deicer 1.5-2.5 parts, idol
Join agent 0.5-1.5 parts, curing agent 0.05-0.15 parts and catalyst 0.05-0.15 parts；
The coupling agent is dodecyl methyl dimethoxysilane HD109 and N-（The aminoethyls of β mono-）- γ-aminopropyl trimethoxy
Base silane KH792,3- TSL 8330 KH540, γ-aminopropyl triethoxysilane KH550, γ-shrink are sweet
A kind of composition in oily ether oxygen propyl trimethoxy silicane KH560.
Further, the silane modified polyether resin is to change by dimethoxysilane and trimethoxy silane mixture
The polyethers obtained after property, molecular weight 10000-15000.
Further, the nano-calcium carbonate is that BET specific surface area is 18-22m2/ g hydrophobic nano calcium carbonate.
Further, the plasticizer is diisooctyl phthalate, diisononyl phthalate, PPG
One or more combinations in N220 and PPG N330.
Further, the deicer is vinyltrimethoxy silane A171,3- mercaptopropyl trimethoxysilane KH591
And one or more combinations in 3- NCO propyl trimethoxy silicanes.
Further, the curing agent is oxazole alkanes curing agent ALT-401 or/and chelant tin C103.The chelant tin
C103 be tetraethyl orthosilicate with it is double（Acetyl group epoxide）The product of dibutyl stannane.
Further, the catalyst is dibutyl tin laurate, tin dilaurate dioctyl tin and ethyl acetoacetate
One or more combinations in titanium.
Chemical reagent described above is commercially available.
The present invention also provides the preparation method of high resiliency silane modified polyether seal glue, comprises the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 0.5-2.0h to 50 DEG C -110 DEG C in the case where vacuum is 0.085-0.095Mpa, mixing speed is 300-500rpm,
Obtain compound；
（2）By step（1）When obtained compound is cooled to 40-45 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum be 0.085-0.095Mpa, mixing speed 300-500rpm, continue stir 0.5-2.0h, obtain polyether seal glue.
Compared with prior art, advantages of the present invention and have the beneficial effect that：
1st, fluid sealant prepared by the present invention has excellent water resistance, elastic recovery rate, weather resistance, mechanical property etc., group
Into composition is relatively simple, cost is cheap.
2nd, the present invention is with long chain type silane coupler dodecyl methyl dimethoxysilane HD109 and silicon different from other
The combination of alkane coupling agent, because it has flexible hydrophobicity long-chain, is improving wellability of the organic matter to filler as coupling agent
Aspect has unique advantage, while can effectively improve the water resistance and elastic recovery rate of fluid sealant, while can be effective
Improve the stability and adhesive property of fluid sealant.
3rd, the present invention is by that with the compounding use of curing agent and catalyst, can be effectively improved the processing fluidity of fluid sealant
Energy.
4th, the inventive method preparation technology is simple, power consumption is low, cost is low, is adapted to industrialized production, has good economy
Benefit and social benefit.
Embodiment
The present invention program is further described below in conjunction with specific embodiment, but is not limited to the protection model of the present invention
Enclose.
Embodiment 1
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Molecular weight is 10000 silane
25 parts of modified polyether resin, nano-calcium carbonate Ca45 part, 1.5 parts of aerosil, diisooctyl phthalate plasticizer 15
Part, 1.5 parts of vinyltrimethoxy silane A171 deicers, dodecyl methyl dimethoxysilane HD109 coupling agents 0.5
Part, N-（The aminoethyls of β mono-）0.5 part of-γ-aminopropyltrimethoxysilane KH792 coupling agents, oxazole alkanes ALT-401 curing agent
0.1 part and 0.15 part of dibutyltin dilaurate catalyst；
Its preparation method, comprise the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 1.5h in the case where vacuum is 0.090Mpa, mixing speed is 500rpm, obtains compound to 60 DEG C；
（2）By step（1）When obtained compound is cooled to 40 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum is 0.090Mpa, mixing speed 500rpm, continues to stir 1.5h, obtains polyether seal glue.
Embodiment 2
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Molecular weight is 12000 silane
30 parts of modified polyether resin, 50 parts of nano-calcium carbonate, 2.0 parts of aerosil, diisononyl phthalate plasticizer 10
Part, 10 parts of PPG N330 plasticizer, 0.5 part of vinyltrimethoxy silane A171 deicers, 3- mercapto propyl group trimethoxies
2.0 parts of base silane KH591 deicers, dodecyl methyl dimethoxysilane HD109 coupling agent 1..0 parts, 3- aminopropyls three
0.2 part of methoxy silane KH540 coupling agents, 0.15 part of chelant tin C103 curing agent and tin dilaurate dioctyl tin catalyst
0.10 part；
Its preparation method, comprise the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 2.0h in the case where vacuum is 0.085Mpa, mixing speed is 300rpm, obtains compound to 80 DEG C；
（2）By step（1）When obtained compound is cooled to 45 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum is 0.085Mpa, mixing speed 300rpm, continues to stir 2.0h, obtains polyether seal glue.
Embodiment 3
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Molecular weight is 15000 silane
20 parts of modified polyether resin, 55 parts of nano-calcium carbonate, 2.5 parts of aerosil, 20 parts of PPG N220 plasticizer,
2.0 parts of 3- NCO propyl trimethoxy silicanes deicer, dodecyl methyl dimethoxysilane HD109 coupling agents
1.0 parts, γ -0.5 part of glycidyl ether oxygen propyl trimethoxy silicane KH560 coupling agents, oxazole alkanes ALT-401 curing agent
0.10 part and 0.10 part of tin dilaurate dioctyl tin catalyst；
Its preparation method, comprise the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 1.5h in the case where vacuum is 0.095Mpa, mixing speed is 500rpm, obtains compound to 100 DEG C；
（2）By step（1）When obtained compound is cooled to 40 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum is 0.095Mpa, mixing speed 500rpm, continues to stir 1.0h, obtains polyether seal glue.
Embodiment 4
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Molecular weight is 10000 silane
35 parts of modified polyether resin, 50 parts of nano-calcium carbonate, 2.0 parts of aerosil, diisooctyl phthalate plasticizer 10
Part, 10 parts of PPG N220 plasticizer, 1.5 parts of vinyltrimethoxy silane A171 deicers, 3- NCOs third
1.0 parts of base trimethoxy silane, 0.5 part of dodecyl methyl dimethoxysilane HD109 coupling agents, the ethoxy of γ-aminopropyl three
0.3 part of base silane KH550 coupling agents, 0.15 part of oxazole alkanes ALT-401 curing agent and tin dilaurate dioctyl tin catalyst
0.05 part and 0.05 part of ethylacetoacetate titanium；
Its preparation method, comprise the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 1.0h in the case where vacuum is 0.085Mpa, mixing speed is 300rpm, obtains compound to 110 DEG C；
（2）By step（1）When obtained compound is cooled to 45 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum is 0.085Mpa, mixing speed 300rpm, continues to stir 1.5h, obtains polyether seal glue.
Embodiment 5
A kind of high resiliency silane modified polyether seal glue, is made up of the raw material of following parts by weight：Molecular weight is 15000 silane
35 parts of modified polyether resin, 50 parts of nano-calcium carbonate, 2.0 parts of aerosil, diisononyl phthalate plasticizer 25
Part, 2.5 parts of vinyltrimethoxy silane A171 deicers, dodecyl methyl dimethoxysilane HD109 coupling agents 0.3
Part, N-（The aminoethyls of β mono-）1.5 parts of-γ-aminopropyltrimethoxysilane KH792 coupling agents, 0.15 part of chelant tin C103 curing agent
With 0.15 part of dibutyltin dilaurate catalyst；
Its preparation method, comprise the following steps：
（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen
Temperature stirs 1.0h in the case where vacuum is 0.090Mpa, mixing speed is 300rpm, obtains compound to 80 DEG C；
（2）By step（1）When obtained compound is cooled to 45 DEG C, deicer, coupling agent, curing agent and catalyst are added,
Vacuum is 0.090Mpa, mixing speed 300rpm, continues to stir 1.0h, obtains polyether seal glue.
Polyether seal glue made from this programme embodiment 1-5 is subjected to detection experiment, wherein tensile strength presses GB/T528-
2009 standards, elongation at break press GB/T528-2009 standards, and elastic recovery rate is tested by GB 13477.17-2002,
Test result is as shown in table 1：
Table 1：The properties of product of various embodiments of the present invention polyether seal glue
Learnt from test result, the modulus of silane modified polyether seal glue prepared by the present invention meets stretch modulus and is less than 0.4MPa
Standard requirement, and there is preferable elastic recovery rate and higher tensile strength.
Claims (8)
- A kind of 1. high resiliency silane modified polyether seal glue, it is characterised in that：It is made up of the raw material of following parts by weight：Silane modified polyether resin 20-35 parts, nano-calcium carbonate 45-55 parts, aerosil 1.5-2.5 parts, plasticizer 15- 25 parts, deicer 1.5-2.5 parts, coupling agent 0.5-1.5 parts, curing agent 0.05-0.15 parts and catalyst 0.05-0.15 parts；The coupling agent is dodecyl methyl dimethoxysilane HD109 and N-（The aminoethyls of β mono-）- γ-aminopropyl trimethoxy Base silane KH792,3- TSL 8330 KH540, γ-aminopropyl triethoxysilane KH550 and γ-shrink A kind of composition in glycerine ether oxygen propyl trimethoxy silicane KH560.
- 2. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The silane modified polyether tree Fat is the polyethers with being obtained after trimethoxy silane mixture modification, molecular weight 10000-15000 by dimethoxysilane.
- 3. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The nano-calcium carbonate is BET specific surface area is 18-22m2/ g hydrophobic nano calcium carbonate.
- 4. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The plasticizer is adjacent benzene two One or more in the isodecyl ester of formic acid two, diisononyl phthalate, PPG N220 and PPG N330 Combination.
- 5. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The deicer is vinyl In trimethoxy silane A171,3- mercaptopropyl trimethoxysilane KH591 and 3- NCO propyl trimethoxy silicane One or more combination.
- 6. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The curing agent is oxazolidine Class curing agent ALT-401 or/and chelant tin C103.
- 7. high resiliency silane modified polyether seal glue according to claim 1, it is characterised in that：The catalyst is two bays One or more combinations in sour dibutyl tin, tin dilaurate dioctyl tin and ethylacetoacetate titanium.
- 8. according to the preparation method of any one of the claim 1-7 high resiliency silane modified polyether seal glues, it is characterised in that： Comprise the following steps：（1）Silane modified polyether resin, nano-calcium carbonate, aerosil, plasticizer are added into high force dispersion mixer, risen Temperature stirs 0.5-2.0h to 50 DEG C -110 DEG C in the case where vacuum is 0.085-0.095Mpa, mixing speed is 300-500rpm, Obtain compound；（2）By step（1）When obtained compound is cooled to 40-45 DEG C, deicer, coupling agent, curing agent and catalyst are added, Vacuum be 0.085-0.095Mpa, mixing speed 300-500rpm, continue stir 0.5-2.0h, obtain polyether seal glue.
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| CN108893061A (en) * | 2018-07-12 | 2018-11-27 | 广西德本仕密封材料有限公司 | A kind of weather-proof dual-component silicane modified polyether seal glue and preparation method thereof |
| CN109233722A (en) * | 2018-08-21 | 2019-01-18 | 新纳奇材料科技江苏有限公司 | A kind of high viscous solid translucent silane-modified joint trimming agent for building and preparation method thereof fastly |
| CN109897589A (en) * | 2019-01-23 | 2019-06-18 | 雨中情防水技术集团有限责任公司 | A kind of high-elastic sealant of environment-friendly type and preparation method thereof |
| CN110204882A (en) * | 2019-06-11 | 2019-09-06 | 广东基地光电有限公司 | A kind of high displacement modified silicon rubber and preparation method thereof |
| CN110373144A (en) * | 2019-08-28 | 2019-10-25 | 广西华纳新材料科技有限公司 | A kind of low modulus height rebound silane modified polyether seal glue of two-component and preparation method |
| CN110408359A (en) * | 2019-08-19 | 2019-11-05 | 浙江皇马科技股份有限公司 | A kind of silane-terminated polyether sealant and its preparation method and application |
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| CN111500240A (en) * | 2020-04-09 | 2020-08-07 | 湖北南北车新材料有限公司 | Silane modified polyether sealant with excellent chemical medium resistance and preparation method thereof |
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| CN113416511A (en) * | 2021-06-09 | 2021-09-21 | 广东工程职业技术学院 | Novel MS sealant for fabricated concrete and preparation method thereof |
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| CN108893061A (en) * | 2018-07-12 | 2018-11-27 | 广西德本仕密封材料有限公司 | A kind of weather-proof dual-component silicane modified polyether seal glue and preparation method thereof |
| CN109233722A (en) * | 2018-08-21 | 2019-01-18 | 新纳奇材料科技江苏有限公司 | A kind of high viscous solid translucent silane-modified joint trimming agent for building and preparation method thereof fastly |
| CN109897589A (en) * | 2019-01-23 | 2019-06-18 | 雨中情防水技术集团有限责任公司 | A kind of high-elastic sealant of environment-friendly type and preparation method thereof |
| CN110204882A (en) * | 2019-06-11 | 2019-09-06 | 广东基地光电有限公司 | A kind of high displacement modified silicon rubber and preparation method thereof |
| CN110204882B (en) * | 2019-06-11 | 2021-06-01 | 广东基地光电有限公司 | High-displacement modified silicone rubber and preparation method thereof |
| CN112094613A (en) * | 2019-06-17 | 2020-12-18 | 南宁学院 | Waterproof sealant for joints of prefabricated external wall panels of prefabricated buildings and production process thereof |
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Application publication date: 20180119 |