CN108865037A - A kind of silane modified polyether seal glue and preparation method thereof, application - Google Patents
A kind of silane modified polyether seal glue and preparation method thereof, application Download PDFInfo
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- CN108865037A CN108865037A CN201710591152.7A CN201710591152A CN108865037A CN 108865037 A CN108865037 A CN 108865037A CN 201710591152 A CN201710591152 A CN 201710591152A CN 108865037 A CN108865037 A CN 108865037A
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- 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
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- 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
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a kind of silane modified polyether seal glues and preparation method thereof, application.The preparation method of silane modified polyether seal glue of the invention includes the following steps：By silane modified polyether resin, powdered whiting, precipitated calcium carbonate, plasticizer, coupling agent and promotor, mixing is vacuumized, under the action of catalyst, deaeration；The plasticizer is diisononyl phthalate.Preparation method of the invention replaces dioctyl phthalate using green plasticization agent diisononyl phthalate, it is more environmentally-friendly to obtain product of the invention, and mechanical property and adhesive property are excellent；Preparation process of the present invention is simple, easily operated, also convenient in construction.
Description
Technical field
The present invention relates to a kind of silane modified polyether seal glues and preparation method thereof, application.
Background technique
Domestic construction sealant is quickly grown, and high-performance building sealant has three classes at present：Silicone, polyurethane and polysulfide.
Wherein, polyurethane sealant has the characteristics that intensity height, tear-proof, soft abrasion-resistant, puncture-resistant, oil resistant, media-resistant corrosion, still
Carbon dioxide is released when solidification makes glue-line generate stomata, and curing rate is poor compared with slow and wet-heat resisting and resistance to ag(e)ing, long-term to store up
It is not good enough to deposit stability；Silicone sealant has quick solidifying, not blistering, can with pore-free material surface secure bond, it is wet-heat resisting, resistance to old
The features such as change is had excellent performance, and storage stability is good, but can application property it is poor, tearing strength is low, not puncture-resistant, and glue-line is also easy to produce oil
Shape dialysis object pollutes concrete, stone material and other ornament materials.
Silicone-modified polyethers sealing material is usually by base polymer (polyoxypropylene of the siliceous alkoxy in both ends), fills out
(such as TiO, CaCO), catalyst [such as Bu Sn (OCOCH), Sn (OCOCH)] and additive composition are expected, because its is low in cost, can room
Temperature vulcanization, good weatherability, and painting can be printed, largely it is used as building sealant and adhesive, and be widely used in various fields.
Silicone-modified polyethers sealing, general formula are as follows：
| Component | Mass number |
| Silane modified polyether | 100 |
| Filler (CaCO3) | 160 |
| Plasticizer (DOP) | 20 |
| Coupling agent | 1 |
| Desiccant | 1.3 |
| Catalyst | 2.0 |
But existing most modified polyurethane sealant viscosity is bigger so that construction get up it is inconvenient, and
Used is most widely used plasticizer phthalic acid dioctyl ester (DOP), for a long time can be carcinogenic with human contact, and not ring
It protects.The status is urgently to be resolved.
Summary of the invention
The present invention is practical, and the technical problem to be solved is that overcome modified polyurethane sealant viscosity ratio in the prior art
Larger, defect not environmentally provides a kind of silane modified polyether seal glue and preparation method thereof, application.This method uses green
Color plasticizer DINP (diisononyl phthalate) replaces DOP, environment-protecting and non-poisonous harmless, and mechanical property and adhesive property are excellent
It is good, it can be applied to the occasion of a variety of needs such as industry, house ornamentation and building general sealing and gluing.
The present invention adopts the following technical solutions to solve above-mentioned technical problem：
The present invention provides a kind of preparation methods of silane modified polyether seal glue comprising following step：Silane is changed
Property polyether resin, powdered whiting, precipitated calcium carbonate, plasticizer, coupling agent and promotor, mixing, vacuumize, catalyst make
Under, deaeration；The plasticizer is DINP (diisononyl phthalate).
The silane modified polyether resin can be the usual resins of this field, and preferred properties parameter is viscosity：
38000mpa.s-45000mpa.s, Cone & Plate viscosity instrument, 25 DEG C, NCO:0 silane modified polyether resin.Described is silane-modified
The dosage of polyether resin can carry out the conventional amount used of such reaction for this field, carry out as long as not influencing reaction, account for original
The mass percent for expecting total amount is preferably 15-40%, and more preferably 25%~40%, such as：25%, 35% or 40%.
The promotor can be the conventional accelerator of this field, optimal ethylene methoxylsilane and/or vinyl second
Oxysilane, more preferable vinyl methoxy silane.The dosage of the promotor can carry out the normal of such reaction for this field
Dosage is advised, is carried out as long as not influencing reaction, the mass percent for accounting for raw material total amount is preferably 0.05~1%, more preferably
It is 0.1%~0.13%, such as：0.1% or 0.13%.
The coupling agent can be the conventional coupling agents of this field, preferably gamma-aminopropyl-triethoxy-silane and/or ethylene
Ethyl triethoxy silicane alkane, more preferable gamma-aminopropyl-triethoxy-silane.The dosage of the coupling agent can carry out this for this field
The conventional amount used of class reaction carries out as long as not influencing reaction, the mass percent for accounting for raw material total amount is preferably 0.5~
3%, such as：0.5%, 2% or 3%.
The powdered whiting is referred to as coarse whiting, is by natural carbonate mineral such as calcite, marble, lime stone mill
It is broken to form, be common powdery inorganic filler, have chemical purity is high, inertia is big, be not easy to chemically react, thermal stability is good,
400 DEG C or less will not decompose, whiteness is high, oil absorbency is low, index of refraction is low, matter is soft, it is dry, be free of the crystallization water, the low wearing valve of hardness
The advantages that small, nontoxic, tasteless, odorless, good dispersion.The dosage of the coarse whiting can carry out the routine of such reaction for this field
Dosage carries out as long as not influencing reaction, the mass percent for accounting for raw material total amount is preferably 5~20%, more preferably
13.8~19%, such as：13.8%, 25% or 19%.Coarse whiting of the invention is purchased from Jiangxi Ao Te fine powder Co., Ltd,
Lot number：1704003, the trade mark：DZ-1250.
The precipitated calcium carbonate is referred to as light calcium, is by artificial synthesized system, and fineness ratio powdered whiting is small, inhales
Oil mass is bigger than powdered whiting, and price is higher than powdered whiting.The dosage of the light calcium can carry out such reaction for this field
Conventional amount used, as long as do not influence reaction carry out, the mass percent for accounting for raw material total amount is preferably 10~35%, more
Preferably 21%~35%, such as：21.5%, 25% or 35%.Light calcium buying of the invention has from Jiangxi special fine powder difficult to understand
Limit company, lot number：1704007, the trade mark：DZ-1290.
The dosage of the plasticizer can carry out the conventional amount used of such reaction for this field, if do not influence to react into
Row, the mass percent for accounting for raw material total amount is preferably 20~35%, and more preferably 20%.
The preferred organo-tin compound of the catalyst, more preferable dibutyl tin dilaurate.The catalyst accounts for original
The mass percent for expecting total amount is preferably 0.1~1.0%, and more preferably 0.2%~0.3%, such as：0.3% or 0.2%.
The preparation method can also further comprise that light stabilizer is added.The light stabilizer can be the normal of this field
Advise light stabilizer, preferably light stabilizer succinic acid and 4- hydroxyl -2,2, polymer, the decanedioic acid of 6,6- tetramethyl -1- piperidine alcohols
Double -2,2,6,6- tetramethyl piperidine alcohol esters and poly- { [6- [(1,1,3,3- tetramethyl butyl) amino]] -1,3,5- triazine -2,4-
[(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two support [(2,2,6,6- tetramethyl -4- piperidyl) imino group]
It is one of (light stabilizer 944) or a variety of, more preferable poly- { [6- [(1,1,3,3- tetramethyl butyl) amino]] -1,3,5- tri-
Piperazine -2,4- [(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two support [(2,2,6,6- tetramethyl -4- piperidyl)
Imino group] }.The dosage of the light stabilizer can carry out the conventional amount used of such reaction for this field, as long as not influencing to react
It carries out, the mass percent for accounting for raw material total amount is preferably 0.1~0.2%, and more preferably 0.1%~0.13%, example
Such as：0.1% or 0.13%.
The mixing can be the conventional mixing of the various materials in this field, and the present invention is preferably by powdered whiting, lightweight carbon
Sour calcium, silane modified polyether resin, plasticizer and promotor put into material cylinder, stir evenly.The stirring can be this field
Convention stir.Preferably, not having subject to particle in material to stir to being uniformly dispersed.The stirring is preferably in double-planet
It is carried out on formula blender.
Described vacuumizing can be carried out by the usual manner of this field, preferably be vacuumized at 100~150 DEG C, more preferably
To be vacuumized at 100~130 DEG C.The time vacuumized can be Conventional Time, such as：1~3 hour.
The preparation method of preferred silane modified polyether seal glue includes the following steps：By light calcium, coarse whiting, silane-modified poly-
Ether resin, coupling agent, plasticizer and promotor put into material cylinder, stir evenly；Light stabilizer is added, high-speed stirred is equal to dispersing
It is even, there is no particle in material；It is vacuumized at 100~150 DEG C, catalyst is added after cooling, stir plastic emitting.Preferably, described
Vacuumize and may also include cooling between the addition catalyst, stop vacuum.
In the present invention, by percentage to the quality, the raw material of the silane modified polyether seal glue be preferably comprised as follows at
Point：
In a better embodiment, the raw material of the silane modified polyether seal glue includes following ingredient：
In another better embodiment, the raw material of the silane modified polyether seal glue includes following ingredient：
The present invention also provides one kind silane modified polyether seal glues as made from above-mentioned preparation method.
The present invention also provides above-mentioned silane modified polyether seal glues on building joint, civil engineering, transport service or
The application of auto manufacturing.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
Percentage in the present invention is the mass percent that each ingredient accounts for raw material total amount.
The positive effect of the present invention is that：DOP is replaced to obtain product of the invention more using green plasticization agent DINP
Add environmental protection, and mechanical property and adhesive property are excellent；Preparation process of the present invention is simple, easily operated, also convenient in construction.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
A kind of preparation method of silane modified polyether seal glue, the method steps are as follows：
(1) it stocks up：It stocks up according to the mass percentage composition of silane modified polyether seal glue；
(2) mixture manufacturing is carried out using double planetary blender：By light calcium, coarse whiting, silane modified polyether resin, coupling
Agent, plasticizer and promotor put into material cylinder, stir evenly；
(3) light stabilizer is added, high-speed stirred does not have particle to being uniformly dispersed in material；
(4) 100~150 DEG C are warming up to, vacuumizes heat preservation 1~3 hour；
(5) 30~60 DEG C are cooled to, vacuum is stopped；
(6) catalyst, after mixing evenly deaeration plastic emitting is added.
Silane modified polyether seal glue, the sealant include following mass percent ingredient：
Each raw material component and mass fraction in 1. embodiment of table
Wherein：The performance parameter of silane modified polyether resin is：Viscosity：38000mpa.s-45000mpa.s Cone & Plate viscosity
Instrument, 25 DEG C, NCO:0；
Plasticizer in embodiment 1-3 and comparative example 1 is DINP, and the plasticizer in comparative example 2 is DOP；
Promotor is vinyl methoxy silane；
Coupling agent is gamma-aminopropyl-triethoxy-silane.
The test of effect data：
Wherein, surface drying time, by GB/T 13477.5-2002-《The 5th part of building sealant method of testing materials：Surface drying
The measurement of time》Middle 8.2B law regulation test；
Tensile strength, 100% stretching strength and elongation rate of tensile failure, by GB/T528-2009-《Vulcanized rubber or thermoplasticity rubber
The measurement of glue tensile stress-strain performance》Regulation test；
Hardness, by GBT 531.1-2008-《Vulcanized rubber or thermoplastic elastomer penetration hardness test method first part：
Shore durometer method (shore hardness)》Regulation test；
Tearing strength, by 529-1991- of GBT《The measurement of vulcanized rubber tearing strength》Regulation test；
100% stretching strength, tensile strength, elongation at break, tearing strength by electronic universal puller system WDW-300 come into
Row test show that the instrument is purchased from testing equipment Co., Ltd of Jinan Huaxing；
Hardness is tested by Shao A hardness tester LX-A, and test apparatus Co., Ltd is had an area of in instrument buying certainly.
The effect data of each embodiment of table 2.
From table 2 it can be seen that the effect in embodiment is compared with comparative example in tensile strength, elongation at break and tearing strength side
Face is greatly improved.
Claims (10)
1. a kind of preparation method of silane modified polyether seal glue, which is characterized in that it includes the following steps：It will be silane-modified poly-
Ether resin, powdered whiting, precipitated calcium carbonate, plasticizer, coupling agent and promotor, mixing, vacuumize, in catalyst action
Under, deaeration；The plasticizer is diisononyl phthalate.
2. preparation method as described in claim 1, which is characterized in that the performance parameter of the silane modified polyether resin is
Viscosity：38000mpa.s-45000mpa.s, Cone & Plate viscosity instrument, 25 DEG C, NCO:0 silane modified polyether resin；
And/or the promotor is vinyl methoxy silane and/or vinylethoxysilane；
And/or the coupling agent is gamma-aminopropyl-triethoxy-silane and/or vinyltriethoxysilane；
And/or the powdered whiting is natural carbonate mineral calcite, marble or lime stone；
And/or the catalyst is organo-tin compound；
And/or it described is mixed into powdered whiting, precipitated calcium carbonate, silane modified polyether resin, plasticizer and promotor
Material cylinder is put into, is stirred evenly；
And/or it described vacuumizes to be vacuumized at 100~150 DEG C.
3. preparation method as claimed in claim 2, which is characterized in that the promotor is vinyl methoxy silane；
And/or the coupling agent is gamma-aminopropyl-triethoxy-silane；
And/or the catalyst is dibutyl tin dilaurate；
And/or the mixing does not have subject to particle in material to stir to being uniformly dispersed；
And/or it described vacuumizes to be vacuumized at 100~130 DEG C.
4. preparation method as described in claim 1, which is characterized in that the silane modified polyether resin accounts for raw material total amount
Mass percent be 15-40%；
And/or the mass percent for accounting for raw material total amount of the promotor is 0.05~1%；
And/or it is 0.5~3% that the coupling agent, which accounts for the mass percent of raw material total amount,；
And/or it is 5~20% that the powdered whiting, which accounts for the mass percent of raw material total amount,；
And/or it is 10~35% that the precipitated calcium carbonate, which accounts for the mass percent of raw material total amount,；
And/or it is 20~35% that the plasticizer, which accounts for the mass percent of raw material total amount,；
And/or it is 0.1~1.0% that the catalyst, which accounts for the mass percent of raw material total amount,.
5. preparation method as claimed in claim 4, which is characterized in that the silane modified polyether resin accounts for raw material total amount
Mass percent is 25%~40%；
And/or it is 0.1%~0.13% that the promotor, which accounts for the mass percent of raw material total amount,；
And/or it is 13.8~19% that the powdered whiting, which accounts for the mass percent of raw material total amount,；
And/or it is 21%~35% that the precipitated calcium carbonate, which accounts for the mass percent of raw material total amount,；
And/or it is 20% that the plasticizer, which accounts for the mass percent of raw material total amount,；
And/or it is 0.2%~0.3% that the catalyst, which accounts for the mass percent of raw material total amount,.
6. preparation method as described in claim 1, which is characterized in that it is steady that the preparation method still further comprises addition light
Determine agent.
7. preparation method as claimed in claim 6, which is characterized in that the light stabilizer is succinic acid and hydroxyl -2 4-,
Double -2,2,6,6- tetramethyl piperidine the alcohol esters of the polymer of 2,6,6- tetramethyl -1- piperidine alcohols, decanedioic acid and it is poly- [6- [(1,1,3,
3- tetramethyl butyl) amino]] -1,3,5- triazine -2,4- [(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two
Support [(2,2,6,6- tetramethyl -4- piperidyl) imino group] one of or it is a variety of；
And/or it is 0.1~0.2% that the light stabilizer, which accounts for the mass percent of raw material total amount,.
8. preparation method as claimed in claim 7, which is characterized in that the light stabilizer is poly- { [6- [(1,1,3,3- tetra-
Methyl butyl) amino]] -1,3,5- triazine -2,4- [(2,2,6,6,-tetramethyl-4-piperidyl) imino group] -1,6- oneself two support
[(2,2,6,6- tetramethyl -4- piperidyl) imino group] }；
And/or it is 0.1%~0.13% that the light stabilizer, which accounts for the mass percent of raw material total amount,.
9. a kind of silane modified polyether seal glue as made from claim 1-8 described in any item preparation methods.
10. a kind of silane modified polyether seal glue as claimed in claim 9 is on building joint, civil engineering, transport service or
The application of person auto manufacturing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109663514A (en) * | 2018-12-29 | 2019-04-23 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of MS glue |
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Application publication date: 20181123 |