CN102093721B - Single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and preparation method thereof - Google Patents
Single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and preparation method thereof Download PDFInfo
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- CN102093721B CN102093721B CN201010280600A CN201010280600A CN102093721B CN 102093721 B CN102093721 B CN 102093721B CN 201010280600 A CN201010280600 A CN 201010280600A CN 201010280600 A CN201010280600 A CN 201010280600A CN 102093721 B CN102093721 B CN 102093721B
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Abstract
The invention particularly relates to single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and a preparation method thereof, which belong to the field of adhesives. The rubber comprises the following components in part by weight: 80 to 120 parts of basic material, 5 to 15 parts of cross linking agent, 10 to 90 parts of thixotropic agent, 10 to 200 parts of filler, 1 to 10 parts of thickening agent and 0.1 to 5 parts of catalyst. The preparation method comprises the following steps of: introducing butanone oximido methoxysilane serving as the cross linking agent and other auxiliary additives into an organic silica polymer serving as the basis material, wherein the cross linking agent consists of methyltrimethoxy silane and 2-butanone oxime; and making the components react in the absence of catalyst at the temperature of between 100 DEG C and 150 DEG C for about 20 hours to obtain the rubber. The rubber has a high vulcanization crosslinking speed and high bonding strength, the effects of insulation, shock resistance, corrosion resistance and the like can be achieved simultaneously, wastes are not produced in a production process, and the rubber belongs to an environmentally-friendly material.
Description
Technical field
The invention belongs to adhesive area, relate in particular to a kind of single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber and preparation method thereof.
Background technology
Room temperature vulcanized silicone rubber is that begin to grow up the sixties in 20th century a kind of is 10000～100000 with suitable molecular mass, and the polydiorganosiloxane of band active end group is the novel organosilicon product of base polymer.Its principal feature is to need not to use complicated mixing and contour machining equipment, at ambient temperature by means of airborne moisture contact or with cross-linking agent component mutually mixing can be sulfided into elastomerics with three-dimensional net structure.
Room temperature vulcanized silicone rubber can be divided into single-component and double component room temperature vulcanization silicon rubber by the physical aspect of product.Single-component room temperature vulcanized Zylox uses technology simple, and construction is preceding without weighing and mixing.Single-component room temperature vulcanized Zylox is different according to the by product that discharges in the vulcanization crosslinking engineering, can be divided into depickling type, ketoxime removing type, dealcoholizing-type again, takes off acid amide type, dehydrogenation type, dehydration-type.
Existing room temperature vulcanized silicone rubber technically, it is slow also to exist vulcanization rate, a little less than the bonding force, characteristics such as insulating property are undesirable, its use properties also are subject to the environmental factors restriction.
Summary of the invention
The present invention is intended to overcome the weak point of prior art, and provides a kind of vulcanization rate fast, and bonding force is strong, good insulation preformance, environmental compatibility ideal single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber.
The present invention also provides a kind of technology for preparing above-mentioned single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber.
For achieving the above object, the present invention is achieved in that
A kind of single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber, it comprises following component: basic thing, linking agent, thixotropic agent, filler, tackifier and catalyzer.
As a kind of preferred version, single-component dealcoholization of the present invention/ketoxime type room temperature vulcanized silicone rubber in weight ratio, comprises following component:
80～120 parts of basis things
5～15 parts of linking agents
10～90 parts of thixotropic agent
10～200 parts of fillers
1～10 part of tackifier
0.1～5 part of catalyzer.
As another kind of preferred version; Basic thing according to the invention is that α, alpha, omega-dihydroxy ZGK 5, α, alpha, omega-dihydroxy gather di-ethyl siloxane or α, alpha, omega-dihydroxy and gather one or more the mixture in the diphenyl siloxane, α, alpha, omega-dihydroxy ZGK 5 that wherein preferred 25 ℃ of following viscosity are 2000-80000mPas.
Further; Linking agent according to the invention can be selected the Diacetylmonoxime methoxylsilane; Diacetylmonoxime methoxylsilane wherein is by methyltrimethoxy silane and 2-butanone oxime, under the condition of catalyst-free; In about 100～150 ℃ TR internal reaction 20h, make, can improve curing speed and bonding strength greatly.
Further; Thixotropic agent according to the invention is one or more the mixture in cyanoethyl Trimethoxy silane, wilkinite, 3# white oil, MTD type silicone oil or the methyl-silicone oil; Make it in application process, all have good thixotropic property, and can not trickle the inclined-plane of wide-angle and the construction of facade.
In addition, filler according to the invention can be selected one or more the mixture in gas-phase silica, precipitated silica, lime carbonate, talcum powder, silicon powder or the Namigai.The preferred gas-phase silica of the present invention is as filler; Because WHITE CARBON BLACK is similar with the backbone structure of Zylox; The molecular chain of Zylox can be adsorbed on the surface of WHITE CARBON BLACK particulate; And the WHITE CARBON BLACK surface contains a large amount of Si-OH base, can form hydrogen bond (physical adsorption) with the Si-O key in the Zylox molecular chain.
Secondly, tackifier according to the invention can be selected a kind of or its mixture in γ-An Bingjisanyiyangjiguiwan or γ-(glycidoxy) propyl trimethoxy silicane.
Once more, catalyzer according to the invention can be selected in dibutyltin diacetate, dibutyl tin laurate or the tetra isopropyl titanate one or more mixture.
The preparation method of above-mentioned single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber, in weight ratio, can implement as follows:
A, 10～200 parts of 80～120 parts of basic things, filler are added in the vacuum kneader, the dehydration blend moves in the planet stirring tank, and is subsequent use;
B, at room temperature adds 5～15 parts of linking agents, 10～90 parts of thixotropic agent, 1～10 part of tackifier, catalyzer in the said planet stirring tank of step a for 0.1～5 part and to mix, and carries out chemical reaction, promptly gets the purpose product.
As a kind of preferred version, among the step a according to the invention, in 80～150 ℃ of temperature, vacuum tightness is 0.06～0.095MPa with basic thing and filler, and dehydration blend 60～300 minutes moves in the planet stirring tank, and is subsequent use; Among the said step b, with mixing in linking agent, thixotropic agent, tackifier and the said planet stirring tank of catalyzer adding step a, be 0.06～0.095MPa in vacuum tightness, rotating speed is that 100～600rpm carried out chemical reaction 30～180 minutes, promptly gets the purpose product.
Dealcoholysis/ketoxime type room temperature vulcanized silicone rubber is a kind of mixed type room temperature vulcanized silicone rubber, and it has overcome long, shortcoming such as adhesion is not good enough ketoxime removing type room temperature vulcanized silicone rubber set time.Simultaneously this Zylox also has insulation, weather-proof, water-fast, dustproof, antifouling, protection against corrosion, premium properties such as shockproof, is not subject to the influence of temperature, change of frequency.
Compared with prior art, the present invention has following advantage:
1, adopting the Diacetylmonoxime methoxylsilane is linking agent, can improve the vulcanization rate and the bonding strength of product.
2, production operation is simple and easy, no generation of waste materials.
3, product easy construction, excellent combination property, each item index all reaches similar products at home and abroad.
Embodiment
Below in conjunction with embodiment the present invention is described further.Protection scope of the present invention not only is confined to the statement of following content.
The present invention is basic thing with α, alpha, omega-dihydroxy ZGK 5; The Diacetylmonoxime methoxylsilane is a linking agent; And be aided with thixotropic agent, filler, tackifier and catalyzer, obtain the single-component dealcoholization that vulcanization rate is fast, bonding strength is big/ketoxime type room temperature vulcanized silicone rubber.
Embodiment 1:
Single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber is characterized in that, in weight ratio, comprises following component:
1 kilogram of α, alpha, omega-dihydroxy ZGK 5
2 kilograms of gas-phase silicas
Diacetylmonoxime methoxylsilane 50 grams
3# white oil 500 grams
γ-An Bingjisanyiyangjiguiwan 100 grams
Dibutyl tin laurate 5 grams.
The preparation method:
Under the drying nitrogen protection; 1 kilogram of α, alpha, omega-dihydroxy ZGK 5 (commodity are called 107 glue, 25 ℃ of viscosity are 80000mPas), 2 kilograms of gas-phase silicas (specific surface area is 150 meters squared per gram) are added in the vacuum kneader; In 120 ℃ of temperature, vacuum tightness is 0.08MPa, dehydration blend 100 minutes; Move in the planet stirring tank, subsequent use.
At room temperature; With Diacetylmonoxime methoxylsilane 50 grams, 3# white oil 500 grams, γ-An Bingjisanyiyangjiguiwan (trade(brand)name KH550) 100 grams; Mix in the dibutyl tin laurate 5 gram adding planet stirring tanks; Vacuum tightness is 0.08MPa, and rotating speed is that 400rpm carried out chemical reaction 60 minutes, makes single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber.
Embodiment 2:
Single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber is characterized in that, in weight ratio, comprises following component:
1 kilogram of α, alpha, omega-dihydroxy ZGK 5
2 kilograms of precipitated silicas
Diacetylmonoxime methoxylsilane 50 grams
Methyl-silicone oil 500 grams
γ-(glycidoxy) propyl trimethoxy silicane 100 grams
Tetra isopropyl titanate 6 grams.
The preparation method:
Under the drying nitrogen protection; 1 kilogram of α, alpha, omega-dihydroxy ZGK 5 (commodity are called 107 glue, 25 ℃ of viscosity are 80000mPas), 2 kilograms of precipitated silicas (specific surface area is 200 meters squared per gram) are added in the vacuum kneader; In 90 ℃ of temperature, vacuum tightness is 0.09MPa, dehydration blend 200 minutes; Move in the planet stirring tank, subsequent use.
At room temperature; With Diacetylmonoxime methoxylsilane 50 grams, methyl-silicone oil (25 ℃ of viscosity are 1000mPas) 500 grams, γ-(glycidoxy) propyl trimethoxy silicane (trade(brand)name KH560) 100 grams; Mix in the tetra isopropyl titanate 6 gram adding planet stirring tanks; Vacuum tightness is 0.09MPa, and rotating speed is that 200rpm carried out chemical reaction 60 minutes, makes single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber.
Embodiment 3:
Single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber is characterized in that, in weight ratio, comprises following component:
1 kilogram of α, alpha, omega-dihydroxy ZGK 5
1 kilogram of precipitated silica
Talcum powder 500 grams
Namigai 500 grams
Diacetylmonoxime methoxylsilane 50 grams
Methyl-silicone oil 500 grams
γ-An Bingjisanyiyangjiguiwan 80 grams
γ-(glycidoxy) propyl trimethoxy silicane 20 grams
Tetra isopropyl titanate 6 grams.
Under the drying nitrogen protection; With 1 kilogram of α, alpha, omega-dihydroxy ZGK 5 (commodity are called 107 glue, 25 ℃ of viscosity are 80000mPas), 1 kilogram of precipitated silica (specific surface area is 200 meters squared per gram), 500 gram talcum powder, 500 gram Namigai, add in the vacuum kneader, in 90 ℃ of temperature; Vacuum tightness is 0.08MPa; Dehydration blend 200 minutes moves in the planet stirring tank, and is subsequent use.
At room temperature, with Diacetylmonoxime methoxylsilane 50 grams, methyl-silicone oil (25 ℃ of viscosity are 1000mPas) 500 grams; γ-An Bingjisanyiyangjiguiwan (trade(brand)name KH550) 80 grams; γ-(glycidoxy) propyl trimethoxy silicane (trade(brand)name KH560) 20 grams mixes in the tetra isopropyl titanate 6 gram adding planet stirring tanks, and vacuum tightness is 0.08MPa; Rotating speed is that 300rpm carried out chemical reaction 30～180 minutes, makes single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber.The performance of products test result is seen table 1.
Table 1 product performance test result
| Project | Standard | Index | Instance 1 | Instance 2 | Instance 3 |
| Density (g/cm3) | GB/T13477.2 | 1.35±0.1 | 1.36 | 1.36 | 1.35 |
| Sag | GB/T13477.6 | <=3 millimeters | 1 | 1 | 1 |
| Surface drying time | GB/T13477.5 | <=3 hours | 8 | 8 | 9 |
| Extrudability | GB/T16776 | <=10 seconds | 7.5 | 7.7 | 7.7 |
| Peel off cementability | GB/T13477.8 | ≥1.0MPa | 1.71 | 1.70 | 1.75 |
Be with being appreciated that; More than about specific descriptions of the present invention; Only be used to the present invention is described and be not to be subject to the described technical scheme of the embodiment of the invention; Those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention, to reach identical technique effect; As long as satisfy the use needs, all within protection scope of the present invention.
Claims (2)
1. single-component dealcoholization/ketoxime type room temperature vulcanized silicone rubber is characterized in that, in weight ratio, comprises following component:
Said basic thing is that α, alpha, omega-dihydroxy ZGK 5, α, alpha, omega-dihydroxy gather di-ethyl siloxane or α, alpha, omega-dihydroxy and gather one or more the mixture in the diphenyl siloxane;
Said linking agent is the Diacetylmonoxime methoxylsilane;
Said thixotropic agent is one or more the mixture in cyanoethyl Trimethoxy silane, wilkinite, 3# white oil, MTD type silicone oil or the methyl-silicone oil;
Said filler is one or more the mixture in gas-phase silica, precipitated silica, lime carbonate, talcum powder, silicon powder or the Namigai;
Said tackifier are a kind of or its mixture in γ-An Bingjisanyiyangjiguiwan or γ-(glycidoxy) propyl trimethoxy silicane;
Said catalyzer is one or more a mixture in dibutyltin diacetate, dibutyl tin laurate or the tetra isopropyl titanate.
2. according to the preparation method of the described single-component dealcoholization of claim 1/ketoxime type room temperature vulcanized silicone rubber, it is characterized in that,, implement as follows in weight ratio:
A, 10～200 parts of 80～120 parts of basic things, filler are added in the vacuum kneader, the dehydration blend moves in the planet stirring tank, and is subsequent use;
B, at room temperature adds 5～15 parts of linking agents, 10～90 parts of thixotropic agent, 1～10 part of tackifier, catalyzer in the said planet stirring tank of step a for 0.1～5 part and to mix, and carries out chemical reaction, promptly gets the purpose product;
Among the said step a, in 80～150 ℃ of temperature, vacuum tightness is 0.06～0.095MPa with basic thing and filler, and dehydration blend 60～300 minutes moves in the planet stirring tank, and is subsequent use;
Among the said step b, with mixing in linking agent, thixotropic agent, tackifier and the said planet stirring tank of catalyzer adding step a, be 0.06～0.095MPa in vacuum tightness, rotating speed is that 100～600rpm carried out chemical reaction 30～180 minutes, promptly gets the purpose product.
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| CN109096980A (en) * | 2018-08-27 | 2018-12-28 | 合肥学院 | A kind of temperature sensitive type changes colour environmentally friendly glass cement and preparation method thereof |
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| CN102516931A (en) * | 2011-12-07 | 2012-06-27 | 北京天山新材料技术股份有限公司 | Ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and preparation method thereof |
| CN102924500A (en) * | 2012-10-26 | 2013-02-13 | 湖北新蓝天新材料股份有限公司 | Preparation method of alkoxymethylethylketoxime silane |
| CN103467508B (en) * | 2013-08-22 | 2015-09-30 | 浙江衢州硅宝化工有限公司 | The preparation method of methyl ketone oxime methoxy silane |
| CN105219340A (en) * | 2015-09-09 | 2016-01-06 | 浙江汇杰有机硅股份有限公司 | Pad glue and preparation method thereof exempted from by a kind of heatproof oil resistant organosilicon |
| CN105112007A (en) * | 2015-09-09 | 2015-12-02 | 蓝星（成都）新材料有限公司 | Single-component organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof |
| CN107142074A (en) * | 2017-05-09 | 2017-09-08 | 江苏天辰新材料股份有限公司 | A kind of preparation method of de-oxime type one component room temperature fluid sealant |
| CN109021916A (en) * | 2018-08-13 | 2018-12-18 | 江苏天辰新材料股份有限公司 | A kind of single-component alcohol/ketoxime-removed room temperature vulcanizing silicone rubber and preparation method |
| CN111621155B (en) * | 2020-05-29 | 2022-04-22 | 广州汇纳新材料科技有限公司 | Two-component ketoxime-removing silicone rubber capable of being deeply cured and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173101A (en) * | 2006-10-30 | 2008-05-07 | 比亚迪股份有限公司 | Single-component ketoxime removing type room temperature vulcanized silicone rubber composition |
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| CN101760172A (en) * | 2008-12-24 | 2010-06-30 | 湖北回天胶业股份有限公司 | Single-component dealcoholization-type organic silicon sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173101A (en) * | 2006-10-30 | 2008-05-07 | 比亚迪股份有限公司 | Single-component ketoxime removing type room temperature vulcanized silicone rubber composition |
Non-Patent Citations (1)
| Title |
|---|
| 吕绍良等.酮肟基甲氧基硅烷的合成及其在单组份有机硅密封胶粘剂中的应用.《粘接》.1992,第13卷(第6期),5-7. * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096980A (en) * | 2018-08-27 | 2018-12-28 | 合肥学院 | A kind of temperature sensitive type changes colour environmentally friendly glass cement and preparation method thereof |
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