CN103756630A - Single-component moldproof transparent dealcoholized silicone sealant and preparation method thereof - Google Patents
Single-component moldproof transparent dealcoholized silicone sealant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a single-component moldproof transparent dealcoholized silicone sealant and a preparation method thereof. The single-component moldproof transparent dealcoholized silicone sealant is prepared by adding a mold preventive into a transparent dealcoholized silicone sealant. The sealant is characterized in that the mold preventive is an organic arsenic compound using polyether glycol as a carrier; and on the basis of 100 parts of alkoxyalkyl terminated polysiloxane, the mold preventive is 0.1-2 parts by weight. By using the organic arsenic compound as the mold preventive, the sealant has the advantages of excellent moldproof effect, low smell, yellowing resistance and high deep curing speed on the premise of not influencing the transparency, manufacturability and storage stability of the transparent dealcoholizd silicone sealant.
Description
Technical field
The present invention relates to transparent dealcoholizing-type silicone sealant of a kind of single-component mildew-resistant and preparation method thereof, belong to organosilicon sealant material technology field.
Background technology
Being accompanied by the building fast development of China, there is larger innovation in Architectural Design and technology, and various type materials obtain application at building field.Single-component room temperature vulcanized silicon rubber, claims again silicone sealant, and owing to having, good cold-resistant, heat-resisting, ageing-resistant, waterproof and moistureproofness are very extensive in various construction works and interior decoration application.Yet silicone sealant exists a shortcoming, after solidifying, in the damp and hot environment of height, mould, easily in its surface breeding, causes its surface to produce black patches for a long time, affects the even sealing property of outward appearance own.Thereby ordinary silicon ketone seal gum in kitchen, the application in the contour humidity of bathing room place is restricted, the exploitation of mould-proof-type silicone sealant is also the certainty of application demand.
Some single-component mildew-resistant silicone sealant products on domestic market, easily there is Yellowing in some defects of ubiquity after solidifying for some time.Number of patent application 201010574200.X discloses a kind of mildew-resistant organosilicon sealant.This invention is on 107 glue are the titanium catalysis dealcoholizing-type organosilicon sealant basis of base glue, to add thiazoles mould inhibitor to form, and anti-mold effect is excellent, but thiazoles mould inhibitor easily causes xanthochromia problem in system.And for example number of patent application 200810130693.0 discloses a kind of preparation method of nanometer mildewproof sealing neutral silicone resin, and this invention is on 107 glue are the titanic acid ester catalysis dealcoholizing-type organosilicon sealant basis of base glue, to add nano-Ag particles to form.Mould inhibitor nano-Ag particles has lasting fungicidal properties and good anti-yellowing property, but the titanate catalyst using in system exists the problem of easy xanthochromia in actual use.The preparation method that above-mentioned two patents relate to all could not solve silicone sealant xanthochromia and a mouldy difficult problem simultaneously.
Summary of the invention
For the deficiencies in the prior art, single-component dealcoholization-type silicone sealant providing a kind of transparent, resistance to xanthochromia, mildew resistance excellence and preparation method thereof is provided the technical problem that the present invention solves.
For realizing above-mentioned technical purpose, technical characterictic of the present invention is, this silicone sealant comprises following component, each component by weight:
Described mould inhibitor is for take the organoarsenium compound that polyether glycol is carrier;
Described catalyzer is organic carboxyl acid tin and inner complex thereof.
The polysiloxane of described alkoxyalkyl end-blocking is preferably terminal methyl group dimethoxy polydimethylsiloxane, and its structural formula is:
The integer that wherein n is 100～1500, in the time of 25 ℃, viscosity is 0.8～150Pas, is preferably 5～150Pas.
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the poly-brick oxygen alkane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises the softening agent of 0 part～100 parts, is preferably 20～100 parts.Described softening agent is inertia polysiloxane in the present invention, is preferably the polydimethylsiloxane of methyl blocking, and in the time of 25 ℃, kinematic viscosity is 0.1～20Pas, is preferably 0.1～5Pas
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the polysiloxane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises the gas-phase silica of 5～40 parts, is preferably 15～30 parts.Described gas-phase silica comprises any one in hydrophilic gas-phase silica, hydrophobic type gas-phase silica, and the present invention selects hydrophobic type gas-phase silica, and specific surface area is 100～300m
2/ g, is preferably 100～200m
2/ g.
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the polysiloxane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises the linking agent of 0～8 part, is preferably 3～8 parts.Described linking agent comprises one or more in methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane, vinyltriethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane, is preferably one or more in methyltrimethoxy silane, vinyltrimethoxy silane, phenyltrimethoxysila,e.
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the polysiloxane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises the mould inhibitor of 0.1～2 part, is preferably 0.2～1.8 part, more preferably 0.3～1.5 part.Described mould inhibitor, for take the organoarsenium compound that polyether glycol is carrier, is preferably adjacent aminobenzene arsonic acid, methylarsonic acid zinc, 10, a kind of in the two phenoxazine arsenic of 10-oxo, more preferably 10, the two phenoxazine arsenic of 10-oxo.
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the polysiloxane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises 0.5～5 part of silane coupling agent, is preferably 2～5 parts, more preferably 3 parts.Described silane coupling agent comprises one or more in γ-aminopropyltrimethoxysilane, N-methyl-3-aminopropyl trimethoxysilane, N-β-amine ethyl γ-amine propyl trimethoxy silicane, γ-glycidoxypropyltrime,hoxysilane.
Single-component dealcoholization-type silicone sealant provided by the invention, by weight, the polysiloxane of 100 parts of alkoxyalkyl end-blockings of take is benchmark, comprises 0.1～3 part of catalyzer, is preferably 0.1-1 part, more preferably 0.4 part.Described catalyzer is organic carboxyl acid tin and inner complex thereof, be preferably dibutyl tin dilaurate, dibutyl tin acetate, dioctyl two tin laurates, two (dodecyl sulphur) dibutyl tin, two fourth methyl ethyl diketone tin, dibutyl methyl aceto acetate tin one or more, be preferably a kind of or two or more in dibutyl tin dilaurate, dioctyl two tin laurates, two (dodecyl sulphur) dibutyl tin.
The invention discloses the transparent dealcoholizing-type silicone sealant of a kind of single-component mildew-resistant preparation method, comprise the following steps:
A) under temperature is 60-80 ℃, nitrogen atmosphere, 107 glue that are 20Pas by 100 parts of kinematic viscosity and 1.6-2 part methyltrimethoxy silane fully stir, and react 60-90 minute to obtain 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes;
B) material told step a) being obtained adds softening agent, gas-phase silica successively, under the condition of vacuum tightness >0.09Mpa, stirs 20-30 minute;
C) by told step b) material that obtains adds linking agent, mould inhibitor, silane coupling agent, catalyzer successively, under the condition of vacuum tightness >0.09Mpa, stirs 10-20 minute, obtains the transparent dealcoholizing-type silicone sealant of single component mildew-proof.
Compared with prior art, it is mould inhibitor that the present invention adopts organoarsenic compound, arsonium ion in organoarsenium compound can combine with the mercapto-of zymoprotein in deteriorative microorganism cell effectively, causes that intracellular sulfydryl enzyme is suppressed and inactivation finally reaches the effect of mildew-resistant, sterilization.
It is the carrier of organoarsenic compound that the present invention adopts polyether glycol, can effectively improve the consistency of organoarsenium compound and silicone sealant system, the in the situation that of less addition, guaranteed that silicone sealant has excellent anti-mold effect, reduced the negative impact of organoarsenium compound to silicone adhesive mechanical property, stability in storage.Polyether glycol has the thixotropy of improving seal gum simultaneously, improves the excellent characteristics such as deep layer solidification rate of seal gum.
It is catalyzer that the present invention adopts organic carboxyl acid tin and inner complex thereof, has shortened surface drying time and deep layer set time of seal gum, overcome the adhesive curing of alcohol type slow, solidify after the easy shortcoming such as xanthochromia.Organo-tin compound also has certain sterilization, anti-mold effect simultaneously.
Embodiment
Below by embodiment, the present invention is specifically described; it is important to point out that following examples are that the present invention is further described; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make according to the present invention nonessential this and enters and adjust.
Embodiment 1
By 100 parts of kinematic viscosity, be that 20Pas107 glue adds in stirrer, under logical nitrogen, temperature 60 C condition, adopt 1.6 parts of methyltrimethoxy silanes, carry out end capping 60 minutes, make 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes; Adding kinematic viscosity is that 15 parts of 100 parts of the polydimethylsiloxanes of 5Pas methyl blocking, hydrophobic type gas type white carbon black that specific surface area is 150m2/g stir 25 minutes under vacuum tightness >0.09Mpa condition; Finally add 8 parts of methyltrimethoxy silanes, the polyether glycol of take is carrier 10,0.4 part of 0.8 part of the two phenoxazine arsenic of 10-oxo, 3 parts of γ-aminopropyltrimethoxysilanes, dibutyl tin dilaurate stir under vacuum tightness >0.09Mpa condition makes the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant for 10 minutes, and product performance test result refers to table 1.
Embodiment 2
107 glue that are 20Pas by 100 parts of kinematic viscosity add in stirrer, adopt 2 parts of methyltrimethoxy silanes to carry out end capping 60 minutes under logical nitrogen, temperature 60 C condition, make 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes; Adding kinematic viscosity is that 50 parts of polydimethylsiloxanes, the specific surface area of 2Pas methyl blocking is 150m
225 parts of/g hydrophobic type gas-phase silicas stir 25 minutes under vacuum tightness >0.09Mpa condition; Finally add 5 parts of vinyltrimethoxy silanes, the polyether glycol of take is carrier 10,0.4 part of 1.5 parts of the two phenoxazine arsenic of 10-oxo, 3 parts of N-β-amine ethyl γ-amine propyl trimethoxy silicanes, dioctyl two tin laurate stir under vacuum >0.09Mpa condition makes the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant for 10 minutes, and product performance test result refers to table 1.
Embodiment 3
107 glue that are 20Pas by 100 parts of kinematic viscosity add in stirrer, adopt 2 parts of methyltrimethoxy silanes to carry out end capping 60 minutes under logical nitrogen, temperature 60 C condition, make 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes; Adding kinematic viscosity is that 20 parts of polydimethylsiloxanes, the specific surface area of 0.3Pas methyl blocking is that 12 parts of 200m2/g hydrophobic type gas-phase silicas stir 25 minutes under vacuum tightness >0.09Mpa condition; Finally add 5 parts of phenyltrimethoxysila,e, the polyether glycol of take is carrier 10,0.4 part of 0.3 part of the two phenoxazine arsenic of 10-oxo, 3 parts of N-methyl-3-aminopropyl trimethoxysilane, two (dodecyl sulphur) dibutyl tin stir under vacuum tightness >0.09Mpa condition makes the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant for 10 minutes, and product performance test result refers to table 1.
Embodiment 4
107 glue that are 20Pas by 100 parts of kinematic viscosity add in stirrer, adopt 2 parts of methyltrimethoxy silanes to carry out end capping 60 minutes under logical nitrogen, temperature 60 C condition, make 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes; After add 18 parts of 20 parts of the polydimethylsiloxanes of 0.3Pas methyl blocking, gas-phase silica that specific surface area is 200m2/g to stir 25 minutes under vacuum tightness >0.09Mpa condition; 0.4 part of 3 parts of 1.8 parts of adjacent aminobenzene arsonic acids, the γ-glycidoxypropyltrime,hoxysilane that finally add 5 parts of methyltrimethoxy silanes, the polyether glycol of take is carrier, dibutyl methyl aceto acetate tin stir under vacuum tightness >0.09Mpa condition makes the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant for 10 minutes, and product performance test result refers to table 1
Comparative example 1
107 glue that are 20Pas by 100 parts of kinematic viscosity add in stirrer, adopt 1.6 parts of methyltrimethoxy silanes, carry out end capping 60 minutes under logical nitrogen, temperature 60 C condition, make 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes; Adding kinematic viscosity is that 100 parts of polydimethylsiloxanes, the specific surface area of 5Pas methyl blocking is 150m
215 parts of the hydrophobic type gas-phase silicas of/g stir 25 minutes under vacuum tightness >0.09Mpa condition; Finally add 0.4 part of 8 parts of methyltrimethoxy silane, 3 parts of Y mono-aminopropyl trimethoxysilane, dibutyl tin dilaurate to stir under vacuum tightness >0.09Mpa condition and within 10 minutes, make the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant, product performance test result refers to table 1.
Testing method:
The present invention carries out quantitative measurement by the transparent dealcoholizing-type silicone sealant of the single-component mildew-resistant obtaining, and detailed process is as follows:
1) adopt the national standard that standard No. is GB/T13477 to test surface drying time and the deep layer curing speed of the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant obtaining;
2) national standard that is GB/T528.1998 according to standard No. is tested hardness, tensile strength, elongation, the mildew-resistant grade of the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant obtaining;
3) the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant is placed 24 hours at 100 ℃ to the xanthochromia situation of aging rear observation adhesive tape.
The silicon gel that embodiment 1～4 and comparative example 1 are obtained carries out performance test, and result is referring to table 1, the performance test results that table 1 is silicone sealant.
The performance test results of table 1 silicone sealant
According to example 1 and comparative example 1, fill a prescription to when performance test data contrast, can find out added take that polyether glycol is carrier 10, after the two phenoxazine arsenic of 10-oxo to seal gum surface drying time, mechanical property, xanthochromia without remarkable negative impact, but effectively improved the deep layer curing speed that fungicidal properties has been accelerated glue simultaneously.When example 2 test datas show this mould inhibitor by formula 2 adding proportion, seal gum mildew-resistant grade can reach 0 grade of highest ranking, and also can meet application requiring without other performances of Yellowing.
Note: mildew-resistant grade explanation:
O level---the obvious mildew of nothing under amplifying approximately 50 times;
1 grade---be invisible to the naked eye or be difficult to see mildew, but can obviously see mildew under magnifying glass;
2 grades---naked eyes are obviously seen mildew, in the fraction of coverage of sample surfaces, are 10%～30%;
3 grades---naked eyes are obviously seen mildew, in the fraction of coverage of sample surfaces, are 30%～60%;
4 grades---naked eyes are obviously seen mildew, in the fraction of coverage of sample surfaces, are greater than 60%.
Claims (8)
1. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant, is characterized in that, the formula of sealing glue is by weight ratio:
Described mould inhibitor is for take the organoarsenium compound that polyether glycol is carrier;
Described catalyzer is organic carboxyl acid tin and inner complex thereof.
2. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, is characterized in that, described alkoxyl group alkane
The polysiloxane of base end-blocking is preferably terminal methyl group dimethoxy polydimethylsiloxane, and its structural formula is:
The integer that wherein n is 100～1500, in the time of 25 ℃, viscosity is 0.8～150Pas.
3. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, is characterized in that, described softening agent is inertia polysiloxane, is preferably the polydimethylsiloxane of methyl blocking, and in the time of 25 ℃, kinematic viscosity is 0.1～20Pas.
4. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, is characterized in that, described gas-phase silica comprises any one in hydrophilic gas-phase silica, hydrophobic type gas-phase silica, and its specific surface area is 100～300m
2/ g.
5. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, it is characterized in that, described linking agent comprises one or more in methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane, vinyltriethoxysilane, phenyltrimethoxysila,e, phenyl triethoxysilane.
6. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, is characterized in that, described organoarsenium compound comprises adjacent aminobenzene arsonic acid, methylarsonic acid zinc, 10, any one in the two phenoxazine arsenic of 10-oxo.
7. the transparent dealcoholizing-type silicone sealant of single-component mildew-resistant according to claim 1, it is characterized in that, described organic carboxyl acid tin and inner complex thereof comprise dibutyl tin dilaurate, dibutyl tin acetate, dioctyl two tin laurates, two (dodecyl sulphur) dibutyl tin, stannous octoate, two fourth methyl ethyl diketone tin, dibutyl methyl aceto acetate tin one or more.
8. the transparent dealcoholizing-type silicone sealant of a single-component mildew-resistant preparation method, comprises the following steps:
A) under temperature is 60-80 ℃, nitrogen atmosphere, 107 glue that are 20Pas by 100 parts of kinematic viscosity and 1.6-2 part methyltrimethoxy silane fully stir, and react 60-90 minute to obtain 100 parts of terminal methyl group dimethoxy polydimethylsiloxanes;
B) material told step a) being obtained adds softening agent, gas-phase silica successively, under the condition of vacuum tightness >0.09Mpa, stirs 20-30 minute;
C) by told step b) material that obtains adds linking agent, mould inhibitor, silane coupling agent, catalyzer successively, under the condition of vacuum tightness >0.09Mpa, stirs 10-20 minute, obtains the transparent dealcoholizing-type silicone sealant of single component mildew-proof.
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| CN104232012A (en) * | 2014-10-14 | 2014-12-24 | 泸州北方化学工业有限公司 | Mold-proof silicone sealant and preparation method thereof |
| CN104479608A (en) * | 2014-12-30 | 2015-04-01 | 北京天山新材料技术有限公司 | Environment-friendly mildewproof silicone-modified polyether sealant |
| CN105505296A (en) * | 2015-12-29 | 2016-04-20 | 江苏创景科技有限公司 | Mildew-proof dealcoholization type organic silicon sealant and preparation method thereof |
| CN106010392A (en) * | 2016-05-27 | 2016-10-12 | 滁州斯迈特复合材料有限公司 | Long-lasting, high-humidity and mold-proof silicone sealant |
| CN108179003A (en) * | 2017-12-25 | 2018-06-19 | 广州市白云化工实业有限公司 | The dealcoholized type silicone weatherproof sealant and preparation method thereof of low modulus, high displacement capacity |
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| CN104232012A (en) * | 2014-10-14 | 2014-12-24 | 泸州北方化学工业有限公司 | Mold-proof silicone sealant and preparation method thereof |
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| CN110003843A (en) * | 2019-04-04 | 2019-07-12 | 北京国电富通科技发展有限责任公司 | A kind of electric power composite insulator repair sheets and preparation method thereof |
| CN110003843B (en) * | 2019-04-04 | 2021-10-15 | 北京国电富通科技发展有限责任公司 | Electric composite insulator repairing adhesive and preparation method thereof |
| CN112574255A (en) * | 2019-09-27 | 2021-03-30 | 中国科学院上海有机化学研究所 | Organic arsine-based CDK inhibitor and preparation method and application thereof |
| WO2021057867A1 (en) * | 2019-09-27 | 2021-04-01 | 中国科学院上海有机化学研究所 | Class of cdk inhibitor based on organic arsine, preparation method and application thereof |
| CN112574255B (en) * | 2019-09-27 | 2024-05-10 | 中国科学院上海有机化学研究所 | Organic arsine-based CDK inhibitor and preparation method and application thereof |
| CN111394014A (en) * | 2020-04-30 | 2020-07-10 | 佛山科普茵生物科技有限公司 | Sealant mildew preventive and preparation method thereof |
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