CN104861912A - Monocomponent silane modified polyether sealant being capable of rapid curing at low temperature and preparation method therefor - Google Patents
Monocomponent silane modified polyether sealant being capable of rapid curing at low temperature and preparation method therefor Download PDFInfo
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- CN104861912A CN104861912A CN201410673256.9A CN201410673256A CN104861912A CN 104861912 A CN104861912 A CN 104861912A CN 201410673256 A CN201410673256 A CN 201410673256A CN 104861912 A CN104861912 A CN 104861912A
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Abstract
The invention provides a monocomponent silane modified polyether sealant being capable of rapid curing at a low temperature and a preparation method therefor, and belongs to the monocomponent room temperature curing silane modified sealant technology field. The monocomponent silane modified polyether sealant mainly solves the problems that low temperature curing is low and adhesive positioning time is long. The monocomponent silane modified polyether sealant comprises the following ingredients, by weight, 100 parts of MS polymers, 10-30 parts of plasticizers, 50-100 parts of bulking fillers, 5-25 parts of reinforcing fillers, 0.5-2 parts of ultraviolet ray absorbers, 0.5-2 parts of ultraviolet ray stabilizing agents, 1-5 parts of thixotropic agents, 0.05-2 parts of water removal agents, 1-5 parts of low-molecular coupling agent polymers and 0.5-2 parts of catalysts. Curing time of an adhesive in a low temperature can be shortened, and the sealant is used for a glue application point with an intensity increasing fast. Under conditions of a temperature of 5 DEG C and a humidity of (55+/-5)% RH, a curing speed for 24h is 2.6mm, shearing intensities for 4h 24h and 168h are 0.3MPa, 1.0MPa and 3.8MPa respectively, the destroy modes are all cohesive failure, the low temperature curing effects are very substantial, and the monocomponent silane modified polyether sealant is widely used in track rail transit train side window glass sealing, elevator reinforcement rib bonding, and bonding of industrial fields of vehicle body luggage compartment doors and the like.
Description
Technical field
The invention belongs to single component technical field of polymer materials, quick-setting single component silane modified polyether seal glue and preparation method thereof under being specifically related to a kind of low temperature, this seal gum at low ambient temperatures can fast setting, form good initial bonding force, setting time is short, bonding for vehicle glass, luggage compartment door is bonding, the industrial application such as elevator stiffening web and chamber door is bonding, device fabrication.
Background technology
Elastic sealant has bonding with sealing two kinds of performances, has the sealing of telescopic displacement and bonding for glass, metal, stone material etc.American-European and Japanese, silane modified polyether seal glue just started to be applied to market in the seventies in last century, mainly achieved good development at building field.Domesticly just start to study in the beginning of this century, current home products process of industrialization is slow, and the key distinction is in domestic construction field many uses silicone series seal gum, and silane modified polyether seal glue is more and more extensive in industrial circle application.
Silane modified polyether seal glue has the advantages such as good weathering resistance, weather resistance, bonding popularity, high resistance Displacement-deformation ability, decorations property, low stain, environment friendliness.Modern industry high speed development, proposes requirements at the higher level to supporting seal gum, especially winter, and the curing speed under low temperature is compared to ambient cure speed and seems not enough, directly affects production efficiency.Therefore, under improving low temperature, single component silane modified polyether seal glue curing speed is extremely important.By consulting literatures and patent, there are no the description to single component silane modified polyether seal glue low-temperature performance.
Summary of the invention
Object of the present invention is exactly solidify slow problem for single component silane modified polyether seal glue under above-mentioned low temperature, by lot of experiments, and quick-setting at low temperatures single component silane modified polyether seal glue of one of invention and preparation method thereof.
Technical solution of the present invention is: fast setting single component silane modified polyether seal glue under a kind of low temperature, it is characterized in that comprising MS polymkeric substance, softening agent, extending fillers, reinforced filling, thixotropic agent, UV light absorber, ultra-violet stabilizer, water-removal agent, low molecule coupling agent polymkeric substance, catalyzer, with mass fraction metering, the consumption of each component is as follows:
100 parts, MS polymkeric substance;
Softening agent 10-30 part;
Extending fillers 50-100 part;
Reinforced filling, to be oil-absorption(number) be this reinforced filling >=super-normal structure black 5-25 part of 100ml/100g;
UV light absorber 0.5-2 part;
Ultra-violet stabilizer 0.5-2 part;
Thixotropic agent 1-5 part;
Water-removal agent 0.05-2 part;
Low molecule coupling agent polymkeric substance, this polymkeric substance is at isolated moisture by poly-Union carbide A-162, methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane, and with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, reacting and within 4-6 hour, obtaining low molecule coupling agent polymkeric substance 1-5 part;
Catalyzer 0.5-2 part.
MS polymkeric substance described in technical solution of the present invention is hydrolyzable silylation polyoxytrimethylene ether, hydrolyzable alkyl refers to trimethoxysilyl or methyl dimethoxy oxygen base silyl.
Softening agent described in technical solution of the present invention is phthalate, alkyl sulfonates, low molecular polyether etc.As any one in dioctyl phthalate (DOP), diisononyl phthalate, Di Iso Decyl Phthalate, benzene sulfonamide acid esters, polyether glycol PPG2000-PPG4000.
Extending fillers described in technical solution of the present invention be nano-calcium carbonate, silicon powder any one.
To be oil-absorption(number) be reinforced filling described in technical solution of the present invention >=super-normal structure black of 100ml/100g.
UV light absorber described in technical solution of the present invention is benzotriazole category; Described ultra-violet stabilizer is a kind of oligomeric, vertical structure hindered amine as light stabilizer.
Thixotropic agent described in technical solution of the present invention is any one in polyoxyethylene glycol, polymeric amide, gas-phase silica.
Water-removal agent described in technical solution of the present invention be in vinyltrimethoxy silane, Additive Ti water-retaining agent any one.
Low molecule coupling agent polymkeric substance described in technical solution of the present invention carries out 60 DEG C of-80 DEG C of back flow reaction, the low-molecular(weight)polymer of reaction 4-6 hour gained with gathering in Union carbide A-162, methyltrimethoxy silane, the aminoethylaminopropyl Trimethoxy silane flask device at isolated moisture and with backflow, drying.
Catalyzer described in technical solution of the present invention is any one in dibutyl tin laurate, dibutyl tin acetate, dioctyl tin cinnamic acid tin.
Under a kind of low temperature of the present invention, the technical solution of quick-setting single component silane modified polyether seal glue is: the making method of quick-setting single component silane modified polyether seal glue under a kind of low temperature, is characterized in that comprising the steps:
(1) first 100 parts of MS polymkeric substance, 10-30 part softening agent, 50-100 part extending fillers, 5-25 part reinforced filling, 0.5-2 part UV light absorber, 0. 5-2 part ultra-violet stabilizer are dropped in planetary mixer and stir, be heated to 60 DEG C simultaneously, add the thixotropic agent of 1-5 part again, keep temperature 60-80 DEG C to stir 10min, open vacuum, vacuum tightness is less than-0.095Mpa, continue to stir 30min, then logical water coolant in planetary mixer chuck, is cooled to 35 DEG C, obtains basic mixture;
(2) Union carbide A-162, methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane will be gathered at isolated moisture, and with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, reacting and within 4-6 hour, obtaining low molecule coupling agent polymkeric substance;
(3) 0.05-2 part water-removal agent, 1-5 part low molecule coupling agent polymkeric substance, 0.5-2 part catalyzer are added in the lump in the basic mixture of step (1), open vacuum, vacuum tightness is less than-0.095Mpa, and stir 30min, discharging divides to be filled in polyethylene tube preserves.
Quick-setting single component silane modified polyether seal glue under adopting the inventive method to prepare a kind of low temperature, mainly be applicable to applying glue under cold condition, energy quick position, be mainly used in track traffic motor-car side glass seal, upholstery material bonding, elevator stiffening web is bonding, vehicle body luggage compartment door adhering and sealing, adhering and sealing material is mainly aluminium alloy.
Under low temperature of the present invention, quick-setting single component silane modified polyether seal glue correlated performance test index is curing speed and shearing resistance; Curing speed tester is about 300mm, and the degree of depth has the gradually dark skewed slot of 0 to 10mm, and available polyethylene plastics are made.Appropriate single component silane modified polyether seal glue is extruded in synclinal bend, by doctor blade, do not make there is bubble in glue-line, 5 DEG C, place 24h under (55 ± 5) %RH condition after uncover glued membrane from thinnest part, to uncured adhesion bottom land place, survey this place's groove depth, be curing speed, in mm/24h.
The test piece used is the aluminum alloy sheet of 2mm × 20mm × 75mm, lap width is (9-11) mm, bondline thickness is 2mm, except the colloid that periphery overflows, temperature 5 DEG C, solidify 4h, 24h, 168h respectively under the condition of humidity (55 ± 5) %RH, then under the speed of 50mm/min, test shearing resistance.
The present invention compared with prior art, there is following advantage and effect: the present invention passes through after coupling agent polymerization, significantly reduce the water-content required for coupling agent self hydrolysis, when moisture-curable met by tackiness agent, moisture mainly participates in the crosslinked of MS polymkeric substance itself, significantly improve curing at low temperatures speed, have obvious lifting to the rising of bonding strength simultaneously.Temperature 5 DEG C, 4h, 24h, 168h is solidified respectively under humidity (55 ± 5) %RH condition, shearing resistance reaches 0.3MPa, 1.0MPa, 3.8MPa respectively, failure mode is cohesive failure, temperature 5 DEG C, under humidity (55 ± 5) %RH condition, 24h curing speed reaches 2.6mm/24h, and short-term curing performance is close to the solidification effect of two-pack product.
Embodiment
The following example and comparative example will introduce the present invention more in detail, but the present invention is not limited to this.Wherein, poly-Union carbide A-162 is Hubei Xiantao Blue Sky Chemical Co., Ltd, and methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane are Jingzhou Jianghan Fine Chemical Co., Ltd..Low molecule coupling agent method for producing polymer: 100 parts of poly-Union carbide A-162s, 50 parts of methyltrimethoxy silanes, 100 parts of aminoethylaminopropyl Trimethoxy silanes are added with temperature agent, isolated moisture, with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, reacting and obtaining low molecule coupling agent polymkeric substance for 4-6 hour.
Embodiment 1:
Proportioning: 100 parts of MS polymkeric substance, 10 parts of different certain herbaceous plants with big flowers esters of phthalic acid two, 80 parts of nano-calcium carbonates, 15 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 0.5 part of UV light absorber, 0.5 portion of ultra-violet stabilizer, 5 parts of polymeric amide, 0.05 part of Additive Ti water-retaining agent, 2 parts of low molecule coupling agent polymkeric substance, 1 part of dibutyl tin acetate.
Preparation technology:
(1) first incite somebody to action: 100 parts of MS polymkeric substance, 10 parts of different certain herbaceous plants with big flowers esters of phthalic acid two, 80 parts of nano-calcium carbonates, 15 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 0.5 part of UV light absorber, 0.5 portion of ultra-violet stabilizer drops in planetary mixer and stirs, be heated to 60 DEG C simultaneously, then add 5 parts of polymeric amide, keep temperature 60-80 DEG C to stir 10min, open vacuum, vacuum tightness is less than-0.095Mpa, continues to stir 30min, then logical water coolant in planetary mixer chuck, be cooled to 35 DEG C, obtain basic mixture;
(2) Union carbide A-162, methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane will be gathered at isolated moisture, and with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, reacting and within 4-6 hour, obtaining low molecule coupling agent polymkeric substance;
(3) by 0.05 part of Additive Ti water-retaining agent, 2 parts of low molecule coupling agent polymkeric substance, 1 part of dibutyl tin acetate adds in the basic mixture of step (1) in the lump, open vacuum, vacuum tightness is less than-0.095Mpa, and stir 30min, discharging divides to be filled in polyethylene tube preserves.
Performance test:
1, curing speed.Curing speed tester is about 300mm, and the degree of depth has the gradually dark skewed slot of 0 to 10mm, and available polyethylene plastics are made.Extrude appropriate MS seal gum in synclinal bend, by doctor blade, do not make there is bubble in glue-line, 5 DEG C, place 24h under (55 ± 5) %RH condition after uncover glued membrane from thinnest part, to uncured adhesion bottom land place, survey this place's groove depth, be curing speed, in mm/24h.
2, shearing resistance.The test piece used is the aluminum alloy sheet of 2mm × 20mm × 75mm, and lap width is (9-11) mm, and bondline thickness is 2mm, remove the colloid that periphery overflows, at 5 DEG C, under 50%RH condition, solidify 4h, 24h, 168h respectively, then under the speed of 50mm/min, test shearing resistance.
Embodiment 2:
Proportioning: 100 parts of MS polymkeric substance, 30 parts of benzene sulfonamide acid esters, 100 parts of nano-calcium carbonates, 20 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 1 part of UV light absorber, 1 portion of ultra-violet stabilizer, 1 part of polymeric amide, 2 parts of vinyltrimethoxy silanes, 5 parts of low molecule coupling agent polymkeric substance, 1.5 parts of dibutyl tin acetates.
Preparation technology and testing method are with embodiment 1.
Test result is in table 1.
Embodiment 3:
Proportioning: 100 parts of MS polymkeric substance, 15 parts of polyether glycol PPG2000,50 parts of nano-calcium carbonates, 10 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 1.5 parts of UV light absorber, 1.5 portions of ultra-violet stabilizers, 2 parts of gas-phase silicas, 1 part of Additive Ti water-retaining agent, 3 parts of low molecule coupling agent polymkeric substance, 0.5 part of dibutyl tin acetate.
Preparation technology and testing method are with embodiment 1.
Test result is in table 1.
Embodiment 4:
Proportioning: 100 parts of MS polymkeric substance, 20 parts of polyether glycol PPG4000,90 parts of silicon powders, 25 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 2 parts of UV light absorber, 2 portions of ultra-violet stabilizers, 4 parts of polyoxyethylene glycol, 1.5 parts of Additive Ti water-retaining agents, 1 part of low molecule coupling agent polymkeric substance, 2 parts of dioctyl tin cinnamic acid tin.
Preparation technology and testing method are with embodiment 1.
Test result is in table 1.
Embodiment 5:
Proportioning: 100 parts of MS polymkeric substance, 25 parts of diisononyl phthalate, 85 parts of silicon powders, 25 parts of oil-absorption(number)s are 150ml/100g super-normal structure black, 1 part of UV light absorber, 1 portion of ultra-violet stabilizer, 3 parts of polyoxyethylene glycol, 1 part of Additive Ti water-retaining agent, 4 parts of low molecule coupling agent polymkeric substance, 1 part of dibutyl tin laurate.
Preparation technology and testing method are with embodiment 1.
Test result is in table 1.
Comparative example 1:
Proportioning: 100 parts of MS polymkeric substance, 40 parts of diisononyl phthalate, 40 parts of nano-calcium carbonates, 15 parts of oil-absorption(number)s are 70ml/100g carbon black, 1 part of UV light absorber, 1 portion of ultra-violet stabilizer, 3 parts of polymeric amide, 2 parts of vinyltrimethoxy silanes, 4 parts of coupling agents (2 parts of methyltrimethoxy silanes and 2 parts of aminoethylaminopropyl Trimethoxy silanes), 1 part of dibutyl tin acetate.
Preparation technology:
(1) first incite somebody to action: 100 parts of MS polymkeric substance, 40 parts of diisononyl phthalate, 40 parts of nano-calcium carbonates, 15 parts of oil-absorption(number)s are 70ml/100g carbon black, 1 part of UV light absorber, and 1 portion of ultra-violet stabilizer drops in planetary mixer and stirs, be heated to 60 DEG C simultaneously, then add 3 parts of polymeric amide, keep temperature 60-80 DEG C to stir 10min, open vacuum, vacuum tightness is less than-0.095Mpa, continues to stir 30min, then logical water coolant in planetary mixer chuck, be cooled to 35 DEG C, obtain basic mixture.
(2) by 2 parts of vinyltrimethoxy silanes, 4 parts of coupling agents (2 parts of methyltrimethoxy silanes and 2 parts of aminoethylaminopropyl Trimethoxy silanes), 1 part of dibutyl tin acetate adds in the basic mixture of step (1) in the lump, open vacuum, vacuum tightness is less than-0.095Mpa, stir 30min, discharging divides to be filled in polyethylene tube preserves.
Testing method is with embodiment 1.
Test result is in table 1.
Comparative example 2:
Proportioning: 100 parts of MS polymkeric substance, 25 parts of polyether glycol PPG2000,40 parts of nano-calcium carbonates, 10 parts of oil-absorption(number)s are 70ml/100g carbon black, 1 part of UV light absorber, 1 portion of ultra-violet stabilizer, 4 parts of polyoxyethylene glycol, 1 part of Additive TI water-retaining agent, 2 parts of coupling agent aminoethylaminopropyl Trimethoxy silanes, 1 part of dibutyl tin laurate.
Preparation technology and the same comparative example of testing method.
Test result is in table 1.
Claims (11)
1. a quick-setting single component silane modified polyether seal glue under low temperature, is characterized in that its composition comprises by weight percentage:
100 parts of MS polymkeric substance,
10 ~ 30 parts of softening agent,
50 ~ 100 parts of extending fillers,
5 ~ 25 parts of reinforced fillings, to be oil-absorption(number) be this reinforced filling >=super-normal structure black of 100ml/100g,
0.5 ~ 2 part of UV light absorber,
5 ~ 2 portions of ultra-violet stabilizers,
1-5 part thixotropic agent,
0.05 ~ 2 part of water-removal agent,
1 ~ 5 part of low molecule coupling agent polymkeric substance, this polymkeric substance is at isolated moisture by poly-Union carbide A-162, methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane, and with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, react and within 4-6 hour, obtain low molecule coupling agent polymkeric substance
0.5 ~ 2 part of catalyzer.
2. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1, is characterized in that: described MS polymkeric substance is hydrolyzable silylation polyoxytrimethylene ether, hydrolyzable alkyl refers to trimethoxysilyl or methyl dimethoxy oxygen base silyl.
3. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, it is characterized in that: described softening agent is phthalate, alkyl sulfonates or low molecular polyether, any one specifically in dioctyl phthalate (DOP), diisononyl phthalate, Di Iso Decyl Phthalate, benzene sulfonamide acid esters, polyether glycol PPG2000-PPG4000.
4. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described extending fillers is nano-calcium carbonate or silicon powder.
5. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described reinforced filling is the super-normal structure black of oil-absorption(number) >=100ml/100g.
6. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described ultraviolet absorbers is benzotriazole category; Described ultra-violet stabilizer is a kind of oligomeric, vertical structure hindered amine as light stabilizer.
7. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described thixotropic agent is any one in polyoxyethylene glycol, polymeric amide, gas-phase silica.
8. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described water-removal agent is vinyltrimethoxy silane or Additive Ti water-retaining agent.
9. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, it is characterized in that: described low molecule coupling agent polymkeric substance carries out 60 DEG C of-80 DEG C of back flow reaction, the low-molecular(weight)polymer of reaction 4-6 hour gained with gathering in Union carbide A-162, methyltrimethoxy silane, the aminoethylaminopropyl Trimethoxy silane flask device at isolated moisture and with backflow, drying.
10. quick-setting single component silane modified polyether seal glue under a kind of low temperature according to claim 1 and 2, is characterized in that: described catalyzer is any one in dibutyl tin laurate, dibutyl tin acetate, dioctyl tin cinnamic acid tin.
11. 1 kinds, for the preparation of the making method of single component silane modified polyether seal glue quick-setting under low temperature according to claim 1, is characterized in that comprising the steps:
(1) first 100 parts of MS polymkeric substance, 10-30 part softening agent, 50-100 part extending fillers, 5-25 part reinforced filling, 0.5-2 part UV light absorber, 0. 5-2 part ultra-violet stabilizer are dropped in planetary mixer and stir, be heated to 60 DEG C simultaneously, add the thixotropic agent of 1-5 part again, keep temperature 60-80 DEG C to stir 10min, open vacuum, vacuum tightness is less than-0.095Mpa, continue to stir 30min, then logical water coolant in planetary mixer chuck, is cooled to 35 DEG C, obtains basic mixture;
(2) Union carbide A-162, methyltrimethoxy silane, aminoethylaminopropyl Trimethoxy silane will be gathered at isolated moisture, and with carrying out 60 DEG C of-80 DEG C of stirring and refluxing reactions in backflow, dry there-necked flask device, reacting and within 4-6 hour, obtaining low molecule coupling agent polymkeric substance;
(3) 0.05-2 part water-removal agent, 1-5 part low molecule coupling agent polymkeric substance, 0.5-2 part catalyzer are added in the lump in the basic mixture of step (1), open vacuum, vacuum tightness is less than-0.095Mpa, and stir 30min, discharging divides to be filled in polyethylene tube preserves.
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Application publication date: 20150826 |