CN105085864A - Alkoxy silane-terminiated polymer and production technology thereof - Google Patents
Alkoxy silane-terminiated polymer and production technology thereof Download PDFInfo
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- CN105085864A CN105085864A CN201410205270.6A CN201410205270A CN105085864A CN 105085864 A CN105085864 A CN 105085864A CN 201410205270 A CN201410205270 A CN 201410205270A CN 105085864 A CN105085864 A CN 105085864A
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- silane
- alkoxysilane
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Abstract
The invention relates to the technical field of an alkoxy silane-terminiated polymer, especially to a high-strength and low-toxicity alkoxy mixed silanes modified polymer for RTV sealants and adhesives and a production technology thereof. The polymer comprises polyurethane, polyether, polyacrylate or any other linear or cross-linked polymer containing free reactive hydroxyl groups which can react. The ratio of methyl dimethoxy to triethoxy is between 2:8 and 8:2. By controlling quantity of carbamic acid ester to minimize hydrogen bonds, viscosity of the polymer at 25 DEG C is within 20000-30000. In comparison with a trimethoxy silane gamma-silane-terminated polymer, the novel alkoxy silane-terminiated polymer has higher mechanical strength. The problem that a trimethoxy silane-terminated product is sensitive to moisture and has short shelf life is solved.
Description
[technical field]
The present invention relates to alkoxysilane-terminated technical field of polymer, particularly relate to the polymer-modified and production technique of the alkoxyl group mixed silanes of a kind of high strength hypotoxicity RTV seal gum and sizing agent.
[background technology]
Silane-terminated polyether and silane end capped polyurethane polymkeric substance all have report at home and abroad as the raw material of sealing material.In mono component wet solidifying system, substitute isocyanate-terminated urethane, there is the advantage of hypotoxicity and high-weatherability.First-generation bifunctional polymer instead of traditional PU seal gum made based on TDI in Automobile Service windshield seals glue.Because these silane modified polymers are not containing any aromatic functional group, so show the uv-resistant performance of highly significant.First-generation polymkeric substance needs high-content tin-containing catalyst and high monohydroxy-alcohol content of polyether to cause to substitute in large volume building and sizing agent market the possibility of PU prepolymer.
Another polymer design route is that polyurethane prepolymer is by all kinds secondary amino group propyl trimethoxy silicane end-blocking.End-cap product has better trimethoxy cross-linking effect, and output low monohydroxy-alcohol DMC high molecular weight polyether, the polymkeric substance that this method design goes out equally with standard P U prepolymer can use the DIDP fluidizer of high-content.The seal gum produced and sizing agent have high response rate, low tin class catalyst content, the surrogate of the PU prepolymer being.But a very large shortcoming is that polymkeric substance and reaction of moisture activity are higher, storage stability is bad, usually in three to six months, just there will be quality comparison.Simultaneously strict to the ambient moisture control overflow in use procedure, the actual operation requirements of most of seal gum manufacturing enterprise can not be met.This kind of polymer viscosity is usually up to more than 100000mPa.s in addition, needs in prepolymer, use the fluidizer of more than 20% content can use these polymkeric substance in the factory.Fluidizer add the decline that membership causes seal gum tensile strength, the seal gum body tensile break strength that this material is made, generally at below 3Mpa/mm2, can not meet the requirement of strength of industrial sealing and matrix material.
Silicane-modified polyurethane SPUR is also the one of seal gum polymkeric substance, but because the viscosity of product is too high, usually at more than 100000mpa.s, use in the process manufacturing seal gum and have larger difficulty, the dispersion liquid of powder material in resin is difficult to evenly simultaneously, causes seal gum product quality unstable.
It is because the hydrogen atom in carbamate groups in double bond Sauerstoffatom and adjacent polymer chains above nitrogen-atoms defines weak bond hydrogen bond thus add viscosity that PU prepolymer and amino-silane terminated urethane have very high viscosity.Standard method is that the viscosity adding dimethylbenzene and fluidizer reduction polyurethane prepolymer and amino-silane terminated SPUR is beneficial to use, but can affect the intensity of cured glue body.The volatilization of organic solvent also causes certain harm to environment.。
Therefore, for overcoming the deficiency of above-mentioned technology and designing a higher physical strength that has, Trimethoxy silane end-blocking product can be solved to a kind of alkoxysilane-terminated polymkeric substance of moisture-sensitive and shelf lives short problem and production technique, just contriver's problem to be solved.
[summary of the invention]
For the deficiencies in the prior art, the object of this invention is to provide a kind of alkoxysilane-terminated polymkeric substance and production technique thereof, there is higher physical strength, Trimethoxy silane end-blocking product can be solved to moisture-sensitive and shelf lives short problem.
For achieving the above object, the present invention can adopt following technical scheme: a kind of alkoxysilane-terminated polymkeric substance, it comprises these polymkeric substance by urethane, polyethers, polyacrylic ester or other have arbitrarily the linear of the free active hydroxy group that can react or cross-linked polymer.
Further, described polymkeric substance, wherein the ratio of methyl dimethoxy oxygen base and triethoxy is between 2:8 to 8:2.
Further, the described quantity by controlling carbamate reduces the effect of hydrogen bond, make polymkeric substance at 25 DEG C viscosity between 20000-30000.
A production technique for alkoxysilane-terminated polymkeric substance, technique comprises following operation steps,
(1) in well-beaten standard laboratory beaker, the low monohydroxy-alcohol DMC catalysis OH value of 12000 molecular weight of 5KG be 10.0 polyethers react with 45.0gIPDI under a nitrogen atmosphere, detect until NCO group content is lower than 1% with infrared spectra, then add 45.0g3-aminopropyltriethoxy dimethoxysilane;
(2) second reactions steps, remaining OH group and the reaction of 79g3-isocyanato propyl-triethoxysilane, until infrared spectra can't detect remaining NCO group, large needs react 6 hours with under the most frequently used PU catalyst condition at 75 DEG C, under 25 DEG C of conditions, the viscosity of this resin is between 20000-30000mPa.s;
(3) detected at 2242cm-1 without any peak by infrared spectra detector, illustrate there is no remaining NCO group, do not dewater at 25 DEG C, 50% humidity in experimental glass ware, under condition with 1% content tin catalyst catalytic polymer, surface drying time is probably 60 minutes, solidifies after 7 days, and your hardness (A) that continues is general 40.
Compared with prior art, beneficial effect of the present invention is: novel alkoxysilane-terminated polymkeric substance, compared to Trimethoxy silane γ-silane-terminated polymer, there is higher physical strength, the tensile break strength of seal gum can reach more than 5Mpa/mm2, and viscosity is between 20000-30000mPa.s.Solve Trimethoxy silane end-blocking product to moisture-sensitive and shelf lives short problem simultaneously.The water content requirement of process to powder filler manufacturing seal gum is relatively low, is applicable to most of seal gum manufacturer, can make the solvent-free environmental protection type sealing adhesive similar with existing PU colloidality energy like this.
[embodiment]
Below in conjunction with specific embodiment, set forth the present invention further, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values drop on application appended claims limited range equally.
These polymkeric substance by urethane, polyethers, polyacrylic ester or other have arbitrarily the linear of the free active hydroxy group that can react or cross-linked polymer.The different main chain of design alternative is the hardness in order to reach needs after active hydroxy group and trifunctional or two functional groups γ-isocyanatosilanes react, and stretches and elongation.These can be known γ and β and α silane.
Polymkeric substance carries out mixing end-blocking by methyl dimethoxysilane and triethoxyl silane, controls the generation quantity of amino-formate bond, avoid the impact that too much hydrogen bond causes polymkeric substance viscosity to raise in molecular backbone chain.Mix capping group simultaneously and show the mechanical property more strengthened than the polymkeric substance of alone any one group end capping after hardening, reach and more reasonably balance.
These silane-terminated polyether stable performances, can allow client can contain filler (as calcium carbonate) up to 2000ppm moisture with different sorts like this, even can add these fillers after the drying step.Also trimethoxyvinyl silane can be used to carry out simple chemical seasoning to filler.
With the low-viscosity polymkeric substance of this uniqueness, we production intensity can manufacture seal gum higher than with trimethoxy silylation terminated polymer, possess the advantage not containing solvent and objectionable constituent simultaneously.We demonstrate some characteristics of this invention on the basis do not limited below.
The Silante terminated mixture A of mixed oxyalkyl
In well-beaten standard laboratory beaker, the low monohydroxy-alcohol DMC catalysis OH value of 12000 molecular weight of 5KG be 10.0 polyethers react with 45.0gIPDI under a nitrogen atmosphere.Detect until NCO group content is lower than 1% with infrared spectra, then add 45.0g3-aminopropyltriethoxy dimethoxysilane.Second reactions steps, remaining OH group and the reaction of 79g3-isocyanato propyl-triethoxysilane, until infrared spectra can't detect remaining NCO group.About needs react 6 hours with under the most frequently used PU catalyst condition at 75 DEG C.Under 25 DEG C of conditions, the viscosity of this resin is probably between 20000-30000mPa.s.
Detect at 2242cm-1 without any peak by infrared spectra detector, illustrate there is no remaining NCO group.Under do not dewater (in experimental glass ware 50% humidity) condition with 1% content tin catalyst catalytic polymer at 25 DEG C, surface drying time is probably 60 minutes.Solidify after 7 days, your hardness (A) that continues is general about 40.
The sealant formula that mixed polymer A makes
When a manufacturers does not have powder drying equipment but to want to make seal gum by this legal system, use the 5L laboratory planetary mixer of standard, under logical nitrogen vacuum low-pressure condition, some sealant specimen can be manufactured with mixed polymer A.Detect calcium carbonate moisture content higher than 2000ppm.
Basic components is in units of part and adjust according to used mixing tank.
Hybrid resin A150 part
Vinyl silanes 1 part
Takehara light calcium carbonate 100 parts
Omyacarb water-ground limestone 100 parts
Titania coating level 50 parts
Silane coupling agent KH7924 part
Tin catalyst 1 part
TinuivinB753 part
AerosilR2024 part
Methyl alcohol 1 part
The mechanical property of the industrial seal gum using mixed polymer A to make.
Surface drying time 15 minutes
Viscosity cp160000
The special test of droop (mm) 0.0 client
Volatile organic matter 1.10% loses
SGg/cm31.41
Tensile strength 5.1n/mm2
Elastic stretching %350%
Continue your hardness (A) 55
Concrete sticking power 95% had cohesive force after 30 days
Stability under high density polyethylene(HDPE) general thickness condition more than 12 months
Although illustrate and describe the main scheme for implementing said method of this patent here, be not intended to describe institute's likely purposes of this patent.More describe and how to use this Macroscopic single crystal hypotoxicity and the PU prepolymer substitute with commercial viability.These examples display seal gum performance is similar to the PU seal gum based on TDI isocyanic ester.
Claims (4)
1. an alkoxysilane-terminated polymkeric substance, its feature is being: it comprises these polymkeric substance by urethane, polyethers, polyacrylic ester or other have arbitrarily the linear of the free active hydroxy group that can react or cross-linked polymer.
2. a kind of alkoxysilane-terminated polymkeric substance according to claim 1, its feature is being: described polymkeric substance, and wherein the ratio of methyl dimethoxy oxygen base and triethoxy is between 2:8 to 8:2.
3. a kind of alkoxysilane-terminated polymkeric substance according to claim 1, its feature is being: the described quantity by controlling carbamate reduces the effect of hydrogen bond, make polymkeric substance at 25 DEG C viscosity between 20000-30000.
4. an alkoxysilane-terminated polymer production process, is characterized in that: technique comprises following operation steps,
(1) in well-beaten standard laboratory beaker, the low monohydroxy-alcohol DMC catalysis OH value of 12000 molecular weight of 5KG be 10.0 polyethers react with 45.0gIPDI under a nitrogen atmosphere, detect until NCO group content is lower than 1% with infrared spectra, then add 45.0g3-aminopropyltriethoxy dimethoxysilane;
(2) second reactions steps, remaining OH group and the reaction of 79g3-isocyanato propyl-triethoxysilane, until infrared spectra can't detect remaining NCO group, large needs react 6 hours with under the most frequently used PU catalyst condition at 75 DEG C, under 25 DEG C of conditions, the viscosity of this resin is between 20000-30000mPa.s;
(3) detected at 2242cm-1 without any peak by infrared spectra detector, illustrate there is no remaining NCO group, do not dewater at 25 DEG C, 50% humidity in experimental glass ware, under condition with 1% content tin catalyst catalytic polymer, surface drying time is probably 60 minutes, solidifies after 7 days, and your hardness (A) that continues is general 40.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279614A (en) * | 2016-08-30 | 2017-01-04 | 江苏凯伦建材股份有限公司 | A kind of silicane-modified polyurethane fluid sealant performed polymer and preparation method thereof and fluid sealant |
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
| CN110734730A (en) * | 2018-07-20 | 2020-01-31 | 东莞市博君来胶粘材料科技有限公司 | silane modified polyether two-component sealant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101535360A (en) * | 2006-09-01 | 2009-09-16 | 莫门蒂夫性能材料股份有限公司 | Solid polymeric substrate having adherent resin component derived from curable silylated polyurethane composition |
| CN102408870A (en) * | 2011-08-16 | 2012-04-11 | 北京天山新材料技术股份有限公司 | Sealant of silane-terminated polymer and preparation method thereof |
-
2014
- 2014-05-15 CN CN201410205270.6A patent/CN105085864A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101535360A (en) * | 2006-09-01 | 2009-09-16 | 莫门蒂夫性能材料股份有限公司 | Solid polymeric substrate having adherent resin component derived from curable silylated polyurethane composition |
| CN102408870A (en) * | 2011-08-16 | 2012-04-11 | 北京天山新材料技术股份有限公司 | Sealant of silane-terminated polymer and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279614A (en) * | 2016-08-30 | 2017-01-04 | 江苏凯伦建材股份有限公司 | A kind of silicane-modified polyurethane fluid sealant performed polymer and preparation method thereof and fluid sealant |
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
| CN110734730A (en) * | 2018-07-20 | 2020-01-31 | 东莞市博君来胶粘材料科技有限公司 | silane modified polyether two-component sealant and preparation method thereof |
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
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Application publication date: 20151125 |