CN108774477A - A kind of plasticizer and preparation method thereof for silicon substrate fluid sealant - Google Patents
A kind of plasticizer and preparation method thereof for silicon substrate fluid sealant Download PDFInfo
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- CN108774477A CN108774477A CN201810635468.6A CN201810635468A CN108774477A CN 108774477 A CN108774477 A CN 108774477A CN 201810635468 A CN201810635468 A CN 201810635468A CN 108774477 A CN108774477 A CN 108774477A
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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
- C09J11/08—Macromolecular additives
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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
- 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
Abstract
The present invention relates to a kind of plasticizer based on silicon substrate fluid sealant, are made of the component including following parts by weight：100 parts of white oil, 20~50 parts of fatty-acid monoester, 0.5~2 part of organo-tin compound.The invention further relates to the preparation methods of the plasticizer.The plasticizer of the present invention is used for silicon substrate fluid sealant, not only there is good tensile strength and elongation at break, but also the modulus of silicon substrate fluid sealant will not reduce, permeability is not easy after use, and there is good heat resistance.
Description
Technical field
The present invention relates to flame-retardant high-molecular field of compound material, and in particular to a kind of plasticizer for silicon substrate fluid sealant,
And the preparation method of the plasticizer.
Background technology
Silicon substrate fluid sealant includes silicone sealant and MS (silane modified polyether) glue two major classes.Wherein, silicone sealant is
Using dimethyl silicone polymer as primary raw material, it is aided with the components such as crosslinking agent, filler, plasticizer, coupling agent and catalyst, in vacuum
The paste mixed under state.The bonding force of silicone sealant is strong, tensile strength is big, while having weatherability, antivibration again
Property, it is moisture-proof and adapt to the big feature of cold and hot variation.In addition its wide applicability can be realized between most of building material products
Bonding, therefore application value is very big.
MS polymer is a kind of cross-linked polymer based on silane-terminated polyether.MS polymer-based products are free of silicone component
And solvent, be free of polyurethanyl group, tasteless environmental protection.The intrinsic elasticity of MS adhesive and fluid sealant is absorbable and compensation dynamic carries
Lotus uniformly transfers stress, prevents material premature fatigue, MS sills from can realize the bonding between a variety of base materials.
Above two silicon substrate fluid sealant all has stronger cementability, is used widely in building trade.In contrast,
Silicone sealant can release the substances such as formaldehyde, VOC (volatile organic matter), harm health because containing solvent.MS glue is free of first
Aldehyde and isocyanates, it is solvent-free, it is non-toxic and tasteless, it is most environmentally friendly building adhesive product.
White oil or methyl-silicone oil are often added in actual use, in silicon substrate fluid sealant as plasticizer, are stretched with reaching to improve
The effect of intensity and elongation at break, but be easy to make the reduction of colloid modulus, it is easy permeability, certain base materials are polluted, even
The caking property of silicon substrate fluid sealant can be reduced, it is therefore desirable to develop new plasticizer.
In consideration of it, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of plasticizer based on silicon substrate fluid sealant.
The second object of the present invention is to provide the preparation method of above-mentioned plasticizer.
To achieve the above object, technical scheme is as follows：
The present invention relates to a kind of plasticizer based on silicon substrate fluid sealant, are made of the component including following parts by weight：
100 parts of white oil, 20~50 parts of fatty-acid monoester, 0.5~2 part of organo-tin compound.
Preferably, the plasticizer is made of the component including following parts by weight：100 parts of white oil, fatty-acid monoester 29~
45 parts, 1~1.5 part of organo-tin compound.
Preferably, the fatty-acid monoester is C4~C18 fatty acid methyl esters.
Preferably, the organo-tin compound is selected from stannous octoate, butyric acid tin, dibutyltin diacetate, two sad two fourths
At least one of Ji Xi, dibutyl tin laurate.
Preferably, polyethers is also contained in the plasticizer, the preferably described polyethers is polyglycol ether.
Preferably, the dosage of the polyethers is 10~20 parts by weight.
Preferably, phthalic acid ester is not contained in the plasticizer.
The invention further relates to the preparation methods of the plasticizer, include the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, organic amine is added, continues 1~2h of insulation reaction；
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains the increasing
Mould agent.
Preferably, the method carries out under conditions of being passed through protection gas.
When containing polyethers in the plasticizer, the preparation method of the plasticizer includes the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, polyethers is added, continues 1~2h of insulation reaction；
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains the increasing
Mould agent.
Beneficial effects of the present invention：
Compared with prior art, the plasticizer of the present invention is used for silicon substrate fluid sealant, not only there is good stretch by force
Degree and elongation at break, and the modulus of silicon substrate fluid sealant will not reduce, and permeability is not easy after use, and have good heat resistance
Energy.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, technical scheme of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
The present embodiments relate to a kind of plasticizer based on silicon substrate fluid sealant, by the component system for including following parts by weight
At：
100 parts of white oil；
20~50 parts of fatty-acid monoester, preferably 29~45 parts；
0.5~2 part of organo-tin compound, preferably 1~1.5 part.
Wherein, white oil also known as paraffin oil, white oil or mineral oil.It is the mixture of the refining liquid hydrocarbon obtained by oil, it is main
It to be the mixture of saturation cycloalkane and alkane.Its main body as plasticizer has good oxidation stability and chemistry
Stability, it is colourless, tasteless, do not corrode fiber textile.Kinematic viscosity of the white oil at 40 DEG C for plasticizer is generally
2mm2/ s to 22mm2/s。
In one embodiment of the invention, fatty-acid monoester is C4~C18 fatty acid methyl esters, and more preferable carbon atom number is
14~18 fatty acid methyl ester.It is good with the compatibility of white oil, and volatility is low, and migration is small, non-toxic and tasteless, has good light
Stability and thermal stability.Since it is in a liquid state at normal temperatures, white oil viscosity can be neutralized, improve each component in plasticizers
Dispersibility.Therefore the addition of fatty-acid monoester cannot be excessive, otherwise can improve the mobility of plasticizer and silicon substrate fluid sealant, nothing
Method realizes non-horizontal surface operation.
In one embodiment of the invention, organo-tin compound is selected from stannous octoate, butyric acid tin, oxalic acid dibutyl
At least one of tin, two sad dibutyl tins, dibutyl tin laurate.In the preparation process of plasticizer, organotin
It is as catalyst to close object, and main there are two the effects of aspect：(1) accelerate crosslinking curing at room temperature, shorten hardening time.(2)
Make sizing material obtained that there is good bin stability.In solidification, stannous octoate is than dibutyltindilaurate catalyzed activity
Greatly, if the two is used in compounding, effect is better than being used alone, and can take into account reaction speed and curing rate.Due to Bivalent Tin
Use nitrogen protection when closing object easily by oxygen in air and steam oxidation and decomposition, therefore storing, it is necessary to seal, avoid high temperature with
Excessive humidity declines or is failed to prevent activity.The most common catalyst of MS glue and silicone sealant is di lauric dibutyl
Tin.
In one embodiment of the invention, also contain polyethers in plasticizer, be with ethylene oxide, propylene oxide, epoxy
Butane etc. is raw material, under the action of catalyst open loop homopolymerization or copolymerization linear polymer obtained.Common polyethers is poly- second two
Alcohol ether.Polyethers is sticky transparency liquid, and property is relatively stable, nontoxic, non-corrosive, good with most organic matter intermiscibilities,
For non-flammable explosives.With the increase of molecular weight, the viscosity of polyethers ramps.It is preferable to use molecular weight be 3000~
8000 polyethers uses it for having lubrication, anti-bubble and heat-resisting freexing tolerance energy well in plasticizer.Since polyethers dissolves in
Water, content in plasticizers cannot be too high, it should in 15 weight % hereinafter, i.e. the dosage of polyethers in the feed is 10~20 weights
Measure part.
Phthalic ester plasticizer is a kind of most popular plasticizer.However this substance is in human body points
Systemic adverse is secreted, there is also carcinogenic risks.Country has made laws to limit and use in current major part developed country and partial development
Phthalic ester plasticizer.Therefore the present invention does not preferably contain phthalic acid ester in plasticizers.The meaning of " being free of "
For the quality relative to plasticizer, plasticizer includes the phthalic acid ester that mass content is less than 1%, and preferably smaller than 0.5%, more
Preferably smaller than 0.1%.
The embodiment of the present invention further relates to the preparation method of the plasticizer, includes the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, organic amine is added, continues 1~2h of insulation reaction.
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains plasticizer.
Above-mentioned reaction carries out under conditions of being passed through protection gas.
When containing polyethers in plasticizer, the preparation method of the plasticizer includes the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, polyethers is added, continues 1~2h of insulation reaction.
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains plasticizer.
The main function of plasticizer is the secondary bond (i.e. Van der Waals force) weakened between polymer molecule, to increase polymerization
The mobility of object strand reduces the crystallinity of polymer molecular chain, that is, increases the plasticity of polymer.Show as polymer
Hardness, modulus, softening temperature and brittle temperature decline, and elongation, flexibility and flexibility improve.Add in silicon substrate fluid sealant
Enter plasticizer, its mobility can be increased, reduce hardness, adjustment modulus.But excessive plasticizer not only results in plasticizer
Migration and exudation, can also influence the droop and mechanical property of fluid sealant.
The preparation method of silicone sealant and MS glue is essentially identical, including：The addition of performed polymer, plasticizer and white carbon is stirred
It mixes in kettle, is performed under heating conditions and is dispersed with stirring, be dehydrated, remaining auxiliary agent is added after being cooled to room temperature, carried out after sizing material is made
Packaging.
Embodiment 1
The preparation of plasticizer
(1) under nitrogen protection, white oil is heated to 50 DEG C, organo-tin compound is added thereto, be warming up to 55 DEG C instead
After answering 40min, polyethers is added, continues insulation reaction 2h；
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 65 DEG C of reaction 2h, obtains plasticizer.Each material
Ingredient and parts by weight be shown in Table 1.
Table 1
In table 1, "-" expression is not present.
In comparative example 1-1 ', plasticizer uses White Mineral Oil.
Above-described embodiment 1-1 to 1-5 and comparative example 1-1 ' plasticizer prepared are used for silicone sealant, specially
In high speed reaction kettle, α, 100 parts by weight of alpha, omega-dihydroxy polydimethyl siloxane, 15 parts by weight of plasticizer and three oxidations are added
Two iron, 1 parts by weight carry out high speed dispersion, and 10 parts by weight of crosslinking agent methyl tributanoximo silane and white carbon 50 are added after 20min
Parts by weight are eventually adding 20 parts by weight of 0.5 parts by weight of titanate chelate and phosphate flame retardant, and silicon is obtained after reacting 30min
Ketone seal gum.
According to professional standard, the silicone sealant that above-described embodiment and comparative example are prepared is tested for the property, and is surveyed
Test result is shown in Table 2.
Table 2
As known from Table 1, embodiment 1-1 not only has good tensile strength and elongation at break, but also silicon substrate fluid sealant
Modulus will not reduce, be not easy permeability after use, and there is good heat resistance.
The fatty-acid monoester content of embodiment 1-2 is higher, and the content of polyether of embodiment 1-4 is higher.With embodiment 1-1 phases
Than not only above-mentioned test parameter decreases, and is easier to ooze out after use.
Embodiment 1-3 has used bicomponent catalyst, there is smaller improvement to the performance of plasticizer.
Polyethers is not used in embodiment 1-5, and above-mentioned performance is declined, but still is better than comparative example 1-1 '.
Above-described embodiment 1-1 to 1-5 and comparative example 1-1 ' plasticizer prepared are used for MS fluid sealants, specially existed
In planet stirring machine barrel, 100 parts by weight of MS polymer, 45 parts by weight of plasticizer, 135 parts by weight of nano-calcium carbonate, antioxygen is added
1 parts by weight of agent carry out high speed dispersion, 3 parts by weight of silane coupling agent are added after dehydrated cooled, after being stirred evenly under vacuum condition
Obtain MS fluid sealants.The MS fluid sealants that embodiment and comparative example obtains are tested according to the record of table 2.
Test result is similar for silicone sealant to by the plasticizer, i.e., embodiment 1-1 and 1-3 shows best drawing
Intensity, elongation at break and modulus are stretched, and is not easy permeability after.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of plasticizer based on silicon substrate fluid sealant, which is characterized in that be made of the component including following parts by weight：White oil
100 parts, 20~50 parts of fatty-acid monoester, 0.5~2 part of organo-tin compound.
2. plasticizer according to claim 1, which is characterized in that the plasticizer is by including the component systems of following parts by weight
At：100 parts of white oil, 29~45 parts of fatty-acid monoester, 1~1.5 part of organo-tin compound.
3. plasticizer according to claim 1 or 2, which is characterized in that the fatty-acid monoester is C4~C18 fatty acid methyls
Ester.
4. plasticizer according to claim 1 or 2, which is characterized in that the organo-tin compound is selected from stannous octoate, fourth
At least one of sour tin, dibutyltin diacetate, two sad dibutyl tins, dibutyl tin laurate.
5. plasticizer according to claim 1 or 2, which is characterized in that also contain polyethers in the plasticizer, it is preferably described
Polyethers is polyglycol ether.
6. plasticizer according to claim 5, which is characterized in that the dosage of the polyethers is 10~20 parts by weight.
7. plasticizer according to claim 1, which is characterized in that do not contain phthalic acid ester in the plasticizer.
8. according to the preparation method of any one of Claims 1-4 the plasticizer, which is characterized in that include the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, organic amine is added, continues 1~2h of insulation reaction；
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains the plasticizer.
9. according to the method described in claim 8, it is characterized in that, the method carries out under conditions of being passed through protection gas.
10. according to claim 5 or the preparation method of 6 the plasticizers, which is characterized in that include the following steps：
(1) white oil is heated to 45~55 DEG C, organo-tin compound is added thereto, be warming up to 55~60 DEG C reaction 30~
After 60min, polyethers is added, continues 1~2h of insulation reaction；
(2) fatty-acid monoester is added into above-mentioned reaction system, is warming up to 60~70 DEG C of 2~3h of reaction, obtains the plasticizer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810635468.6A CN108774477B (en) | 2018-06-20 | 2018-06-20 | Plasticizer for silicon-based sealant and preparation method thereof |
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| CN201810635468.6A CN108774477B (en) | 2018-06-20 | 2018-06-20 | Plasticizer for silicon-based sealant and preparation method thereof |
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| CN108774477A true CN108774477A (en) | 2018-11-09 |
| CN108774477B CN108774477B (en) | 2021-03-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105482769A (en) * | 2016-02-01 | 2016-04-13 | 常州市君成机械有限公司 | Preparation method for modified white oil silicone sealant plasticizer |
| JP2017073299A (en) * | 2015-10-08 | 2017-04-13 | 株式会社ニッペコ | Surface protective agent for electrical contact and electrical contact using the same, and connector |
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2018
- 2018-06-20 CN CN201810635468.6A patent/CN108774477B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017073299A (en) * | 2015-10-08 | 2017-04-13 | 株式会社ニッペコ | Surface protective agent for electrical contact and electrical contact using the same, and connector |
| CN105482769A (en) * | 2016-02-01 | 2016-04-13 | 常州市君成机械有限公司 | Preparation method for modified white oil silicone sealant plasticizer |
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Denomination of invention: The invention relates to a plasticizer for silicon-based sealant and a preparation method thereof Effective date of registration: 20211223 Granted publication date: 20210302 Pledgee: Guangzhou Baiyun Branch of China Construction Bank Co.,Ltd. Pledgor: GUANGZHOU LEISIMAN NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980016117 |
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