CN103320079A - Preparation method of flame retardant single-component silane modified polyether sealant - Google Patents
Preparation method of flame retardant single-component silane modified polyether sealant Download PDFInfo
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- CN103320079A CN103320079A CN2013102907220A CN201310290722A CN103320079A CN 103320079 A CN103320079 A CN 103320079A CN 2013102907220 A CN2013102907220 A CN 2013102907220A CN 201310290722 A CN201310290722 A CN 201310290722A CN 103320079 A CN103320079 A CN 103320079A
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Abstract
The invention discloses a preparation method of a flame retardant single-component silane modified polyether sealant. The flame retardant single-component silane modified polyether sealant comprises an MS premix, a cross-linking agent, a coupling agent and a catalyst, wherein the MS premix comprises 20-60 parts of silane modified polyether, 5-15 parts of plasticizer, 20-40 parts of flame retardant filler, 10-30 parts of reinforcing filler, 0.1-2 parts of thixotropic agent and 0.1-2 parts of functional auxiliaries. The preparation method comprises the following steps: sequentially adding the silane modified polyether, the plasticizer, the flame retardant filler, the reinforcing filler, the thixotropic agent and the functional auxiliaries into a stirring kettle at room temperature, performing vacuum blending for 10-15 minutes, heating to 100-120 DEG C, performing vacuum blending for 1 hour, and performing vacuum cooling to room temperature to get the MS premix; performing vacuum stirring on 80-95 parts of the MS premix and 0.1-3 parts of water remover for 20 minutes, then sequentially adding 0.1-3 parts of cross-linking agent, 0.1-3 parts of coupling agent and 0.1-2 parts of catalyst, and performing vacuum stirring for 20 minutes to get the high-performance flame retardant single-component silane modified polyether sealant which is uniform in dispersion and has a thixotropic property.
Description
Technical field
The present invention relates to a kind of preparation method of flame retardant type single-component silane modified polyether seal glue.
Background technology
" development of single-component silane modified polyether seal glue " that Huitian Glue Ind Co., Ltd., Hubei delivered in October, 2010, prescription is the single-component silane modified polyether seal glue of MS prepolymer 100, softening agent 20～40, calcium carbonate 100～120, thermal silica, silane coupling agent 2～7 and catalyzer 1～2, overcome some defectives of silane seal gum by modification, improved the environment friendliness.
End-silicane-group polyoxytrimethylene (claiming again silane modified polyether (MS-polymer)) is the base polymer of silyl-terminated polyether sealant, in 1979 first by Japanese clock deep pool chemical industry (strain) exploitation listing, and in succession develop silyl-terminated polyether sealant.Obtained Japanese polymer association scientific award in 1980, beginning in 1981 is applied in heavy construction, and obtains good effect.Then, many companies also develop series modified silicone elastic sealant in succession, and this haves laid a good foundation for silyl-terminated polyether sealant obtained later on fast development in 1986.
The over-all properties of silane modified polyether seal glue and the balance of over-all properties be comparative superiority all, shows good weather-proof, weather resistance, high anti-deformational displacement ability, good cohesiveness, covering with paint property, environment friendliness, the advantages such as low staining property and good workability.
The high speed development of modern industry is had higher requirement to the safety and reliability of seal gum, and the development of flame-retardant, silane modified polyether seal glue is a difficult point always.
Summary of the invention
The object of the invention is: the preparation method that a kind of flame retardant type single-component silane modified polyether seal glue is provided.
The object of the invention is achieved through the following technical solutions: a kind of preparation method of flame retardant type single-component silane modified polyether seal glue, comprise MS Preblend, linking agent, coupling agent and catalyzer, and each component is by mass parts,
MS Preblend:
20～60 parts silane modified polyether
5～15 parts softening agent
20～40 parts fire-retardant filler
10～30 parts of reinforced fillings
0.1～2 parts thixotropic agent
0.1～2 parts functional agent,
Described fire-retardant filler is one or more in aluminium hydroxide, magnesium hydroxide, antimonous oxide, zinc borate, melamine cyanurate, the melamine salt;
The end group of described silane modified polyether is the polyoxytrimethylene ether of hydrolyzable silane base, described hydrolyzable silane base is trimethoxysilyl or methyl dimethoxy oxygen base silyl, such as product SAT010, the SAT400 of Japanese KANEKA company, SAT3500, S203H, S303H etc., basic structure is:
Or
Described functional agent is one or more in uv-absorbing agent, photostabilizer, the oxidation inhibitor;
After at room temperature order adds silane modified polyether, softening agent, fire-retardant filler, reinforced filling, thixotropic agent, performance auxiliary agent in the twin shaft planet stirring still, blend is 10～15 minutes under vacuum protection, then be warmed up to 100～120 ℃ of lower vacuum protection blend 1 hour, the vacuum protection borehole cooling namely obtains MS Preblend to room temperature;
The MS seal gum:
80～95 parts MS Preblend
0.1～3 parts water-removal agent
0.1～3 parts linking agent
0.1～3 parts coupling agent
0.1～2 parts of catalyzer,
Described linking agent is one or more in vinyltrimethoxy silane, methyltrimethoxy silane, Union carbide A-162, methyl silicate, tetraethoxy, the positive silicic acid propyl ester;
Described catalyzer is a kind of in dibutyltin diacetate, oxalic acid dioctyl tin, two sad dibutyl tins, stannous octoate, tin acetate, dibutyl tin laurate and the organic tin compound;
Get MS Preblend in twin shaft planet stirring still, add first water-removal agent, vacuum stirring 20 minutes, then order adds linking agent, coupling agent, catalyzer, vacuum stirring 20 minutes, obtaining being uniformly dispersed has thixotropic One component Sealant.Sealing glue has excellent in flame retardance, and cementability is good.
On the such scheme basis, described softening agent is dioctyl phthalate (DOP), phthalic acid two certain herbaceous plants with big flowers esters, phenyl-phosphate class, a kind of in the alkyl phosphate class.
On the such scheme basis, described reinforced filling is nano-calcium carbonate, silicon powder, white carbon black, one or more in the mica powder.
On the such scheme basis, described thixotropic agent is the polymeric amide thixotropic agent, carbon black, white carbon black, hydrogenated castor oil, one or more in the organobentonite.
On the such scheme basis, described water-removal agent is one or more in hexamethyldisilazane, vinyltrimethoxy silane, isocyanates silane coupling agent, the oxazole alkanes coupling agent.
On the such scheme basis, described coupling agent is one or more of γ-aminopropyl triethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyltrimethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane.
Described functional agent is the product of two key chemical industry, comprise in uv-absorbing agent, photostabilizer, the oxidation inhibitor one or more, as: described performance auxiliary agent: CHISORB BP-3, CHISORB BP-12, CHISORB 234, CHISORB 320, CHISORB 326, CHISORB 327, CHISORB 5103, CHISORB 335, CHISORB 1278, CHISORB 66 etc.; The special company of cyanogen product: UV-3638, UV-5411, UV-531, UV-24, UV-1164 etc.; Ciba product: one or more among Tinuvin 99-2, Tinuvin 928, Tinuvin 326, Tinuvin 770, Tinuvin 292, Tinuvin 5050, Tinuvin 5055, Tinuvin 5151, Tinuvin 5060Tinuvin 327, the Tinuvin 329.
Superiority of the present invention is: the seal gum of acquisition has excellent in flame retardance, the characteristics that cementability is good, and preparation method of the present invention is simple, safety, is fit to the adhering and sealing of building, communications and transportation, sun power etc.
Embodiment
The present embodiment provides two kinds of preferred proportion schemes, wherein, and prescription one:
MS Preblend:
MS-polymerS303H
Dioctyl phthalate (DOP)
Aluminium hydroxide, melamine cyanurate
Calcium carbonate
Polymeric amide
CHISORB?234
Tinuvin?770
The MS seal gum:
MS Preblend
Vinyltrimethoxy silane
N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane
Dibutyl tin laurate.
Prescription two:
MS Preblend:
MS-polymerS303H
Phthalic acid two certain herbaceous plants with big flowers esters
Aluminium hydroxide, benzotriazole
Calcium carbonate
Organobentonite
CHISORB?335
Tinuvin?292
The MS seal gum:
MS Preblend
The isocyanic ester Trimethoxy silane
γ-aminopropyltrimethoxysilane
The oxalic acid dioctyl tin.
Prepare burden in the steps below:
After at room temperature order adds silane modified polyether, softening agent, fire-retardant filler, reinforced filling, thixotropic agent, performance auxiliary agent in the twin shaft planet stirring still, blend is 10～15 minutes under vacuum protection, then be warmed up to 100～120 ℃ of lower vacuum protection blend 1 hour, the vacuum protection borehole cooling namely obtains MS Preblend to room temperature; Get partly-premixed material in twin shaft planet stirring still, add first water-removal agent, vacuum stirring 20 minutes, then order adds linking agent, coupling agent, catalyzer, vacuum stirring 20 minutes, obtaining being uniformly dispersed has thixotropic One component Sealant.Sealing glue has excellent in flame retardance, and cementability is good.
Embodiment 1
MS Preblend:
30g?MS-polymerS303H
The 10g dioctyl phthalate (DOP)
30g aluminium hydroxide
7.4g melamine cyanurate
22g calcium carbonate
0.2g polymeric amide
0.2g?CHISORB?234
0.2g?Tinuvin?770
The MS seal gum:
98.2g MS Preblend
0.9g vinyltrimethoxy silane
0.6g N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane
0.3g dibutyl tin laurate.
Embodiment 2
MS Preblend:
27g?MS-polymerS303H
10.2g triphenylphosphate
30g aluminium hydroxide
The 10g magnesium hydroxide
22g calcium carbonate
0.3g polymeric amide
0.25g?CHISORB?BP-12
0.25g?CHISORB?1278
The MS seal gum:
98.2g MS Preblend
0.8g methyltrimethoxy silane
0.6g γ-aminopropyltrimethoxysilane
0.4g oxalic acid dioctyl tin.
Embodiment 3
MS Preblend:
30g?MS-polymerS303H
The 10g dioctyl phthalate (DOP)
30g aluminium hydroxide
7.4g antimonous oxide
The 22g mica powder
0.2g polymeric amide
0.2g?CHISORB?234
0.2g?Tinuvin?770
The MS seal gum:
98.3g MS Preblend
0.6g vinyltrimethoxy silane
0.6g N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane
0.2g γ-glycidyl ether oxygen propyl trimethoxy silicane
0.3g stannous octoate.
Embodiment 4
MS Preblend:
27g?MS-polymerS303H
The 10g dioctyl phthalate (DOP)
The 30g antimonous oxide
7.4g melamine cyanurate
The 25g silicon powder
0.2g polymeric amide
0.1g?Tinuvin?326
0.3g?CHISORB?5103
The MS seal gum:
98.2g MS Preblend
0.9g vinyltrimethoxy silane
0.6g N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane
0.3g tin acetate.
Be noted that for those skilled in the art, under the premise of not departing from the present invention, can also make some improvement and modification, these improvement and modification also should be considered as protection scope of the present invention.
Claims (6)
1. the preparation method of a flame retardant type single-component silane modified polyether seal glue comprises MS Preblend, linking agent, coupling agent and catalyzer, it is characterized in that: each component is by mass parts,
MS Preblend:
20～60 parts silane modified polyether
5～15 parts softening agent
20～40 parts fire-retardant filler
10～30 parts of reinforced fillings
0.1～2 parts thixotropic agent
0.1～2 parts functional agent,
Described fire-retardant filler is one or more in aluminium hydroxide, magnesium hydroxide, antimonous oxide, zinc borate, melamine cyanurate, the melamine salt;
The end group of described silane modified polyether is the polyoxytrimethylene ether of hydrolyzable silane base, and described hydrolyzable silane base is trimethoxysilyl or methyl dimethoxy oxygen base silyl, and basic structure is:
Or
Described functional agent is one or more in uv-absorbing agent, photostabilizer, the oxidation inhibitor;
After at room temperature order adds silane modified polyether, softening agent, fire-retardant filler, reinforced filling, thixotropic agent, performance auxiliary agent in the twin shaft planet stirring still, blend is 10～15 minutes under vacuum protection, then be warmed up to 100～120 ℃ of lower vacuum protection blend 1 hour, the vacuum protection borehole cooling namely obtains MS Preblend to room temperature;
The MS seal gum:
80～95 parts MS Preblend
0.1～3 parts water-removal agent
0.1～3 parts linking agent
0.1～3 parts coupling agent
0.1～2 parts of catalyzer,
Described linking agent is one or more in vinyltrimethoxy silane, methyltrimethoxy silane, Union carbide A-162, methyl silicate, tetraethoxy, the positive silicic acid propyl ester
Described catalyzer is a kind of in dibutyltin diacetate, oxalic acid dioctyl tin, two sad dibutyl tins, stannous octoate, tin acetate, the dibutyl tin laurate;
Get MS Preblend in twin shaft planet stirring still, add first water-removal agent, vacuum stirring 20 minutes, then order adds linking agent, coupling agent, catalyzer, vacuum stirring 20 minutes, obtaining being uniformly dispersed has thixotropic highly effective flame-retardant type single-component silane modified polyether seal glue.
2. the preparation method of flame retardant type single-component silane modified polyether seal glue as claimed in claim 1 is characterized in that, described softening agent is dioctyl phthalate (DOP), phthalic acid two certain herbaceous plants with big flowers esters, phenyl-phosphate class, a kind of in the alkyl phosphate class.
3. the preparation method of flame retardant type single-component silane modified polyether seal glue as claimed in claim 1, it is characterized in that: described reinforced filling is nano-calcium carbonate, silicon powder, white carbon black, one or more in the mica powder.
4. the preparation method of flame retardant type single-component silane modified polyether seal glue as claimed in claim 1, it is characterized in that: described thixotropic agent is the polymeric amide thixotropic agent, carbon black, white carbon black, hydrogenated castor oil, one or more in the organobentonite.
5. the preparation method of flame retardant type single-component silane modified polyether seal glue as claimed in claim 1, it is characterized in that: described water-removal agent is one or more in hexamethyldisilazane, vinyltrimethoxy silane, isocyanates silane coupling agent, the oxazole alkanes coupling agent.
6. the preparation method of flame retardant type single-component silane modified polyether seal glue as claimed in claim 1 is characterized in that: described coupling agent agent is one or more of γ-aminopropyl triethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyltrimethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane.
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| CN103333653A (en) * | 2013-07-12 | 2013-10-02 | 上海魁固塑胶制品有限公司 | Antiflaming one-component modified silane polyether sealant and preparation method thereof |
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| CN103756618A (en) * | 2014-01-10 | 2014-04-30 | 常熟市恒信粘胶有限公司 | Fast curing sealant of silane-modified polyether |
| CN104861912A (en) * | 2014-11-22 | 2015-08-26 | 湖北回天新材料股份有限公司 | Monocomponent silane modified polyether sealant being capable of rapid curing at low temperature and preparation method therefor |
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| CN113637445A (en) * | 2021-07-28 | 2021-11-12 | 杭州之江新材料有限公司 | Silane modified flame-retardant adhesive and preparation method thereof |
| CN113637445B (en) * | 2021-07-28 | 2023-01-03 | 杭州之江新材料有限公司 | Silane modified flame-retardant adhesive and preparation method thereof |
| CN114276769A (en) * | 2022-01-21 | 2022-04-05 | 郑州圣莱特空心微珠新材料有限公司 | Silane modified polyether sealant, preparation method thereof and application thereof in fabricated building |
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| CN114539963A (en) * | 2022-04-01 | 2022-05-27 | 湖北航天化学技术研究所 | Thixotropic silane modified polyether sealant and preparation method thereof |
| CN114539963B (en) * | 2022-04-01 | 2024-01-19 | 湖北航天化学技术研究所 | Thixotropic silane modified polyether sealant and preparation method thereof |
| EP4279555A1 (en) | 2022-05-19 | 2023-11-22 | Bostik SA | Moisture curable composition |
| WO2023222623A1 (en) | 2022-05-19 | 2023-11-23 | Bostik Sa | Moisture curable composition |
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