CN101469067B - Modified silicone rubber and preparation technique thereof - Google Patents
Modified silicone rubber and preparation technique thereof Download PDFInfo
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- CN101469067B CN101469067B CN2009100010093A CN200910001009A CN101469067B CN 101469067 B CN101469067 B CN 101469067B CN 2009100010093 A CN2009100010093 A CN 2009100010093A CN 200910001009 A CN200910001009 A CN 200910001009A CN 101469067 B CN101469067 B CN 101469067B
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- silicone rubber
- modified silicone
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- polyether glycols
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Abstract
The invention belongs to the technical field of adhesive, and discloses a modified silicone rubber and a preparation method thereof. The modified silicone rubber is mainly technically characterized by comprising the following components: 8 to 12 weight portions of polyether diol, 1 to 3 weight portions of isocyanate, and 2 to 5 weight portions of amino silicane. The polyether diol is treated by vacuumizing, heating and degassing, and the isocyanate and the pretreated polyether diol are subjected to chemical reaction and dehydrated and extracted to prepare the modified silicone rubber. Silicone fluid sealant prepared by the silicone rubber can be used for construction in the damp environment, has low cleanliness requirement on an interface, and has the advantage of convenient construction.
Description
Technical field
The invention belongs to technical field of adhesive, and relate to a kind of modified silicone rubber and preparation technology thereof.
Background technology
Silicone rubber is the main raw material of preparation silicone sealant, and silicone sealant is a kind of tackiness agent of excellent property, is widely used in the various engineerings such as expansion joint in bonding, the road engineering of civil engineering, glass.But the silicone sealant by the silicone rubber preparation in use exists following shortcoming: one, sticking and curing mechanism from silicone sealant, construction in a humid environment, silicone sealant can react with airborne water generates before uncured, does not reach the adherent purpose thereby reduce its bond properties; Its two, when silicone sealant was made tackiness agent, bonding interface must be accomplished cleaning surfaces, otherwise can influence the bonding and sealing property of interface; They are three years old, the preparation technology of silicone rubber as the main raw material of preparation silicone sealant, owing to be a kind of scission of link between the silica of silicon-dioxide to be reacted, this reacts wayward and technology more complicated, and thus the storage time of the silicone rubber that generates of technology and silicone sealant thereof general only one year about, exist short problem of storage time.
Summary of the invention
First purpose of the present invention just provides that preparation technology is simple, storage time is long, adhesive effect is good and the modified silicone rubber of easy construction.
Second purpose of the present invention just provides the method for the above-mentioned modified silicone rubber of preparation.
A kind of modified silicone rubber that preparation the present invention proposes is made of the polyether Glycols of 8-12 weight part, the isocyanic ester of 1-3 weight part and the aminosilane ingredient of 2-5 weight part.
The method steps of realizing the above-mentioned a kind of modified silicone rubber of preparation is:
The first step: to the processing of polyether Glycols
Take by weighing polyether Glycols and insert in the reactor, be evacuated to 200-300mmHg and be heated to 90-125 ℃ simultaneously, be incubated venting after 4-8 hour;
Second step: reaction
Take by weighing isocyanic ester in proportion and add in the aforesaid reaction vessel, make it to carry out chemical reaction, and kept 30-50 hour, after the viscosity of resultant of reaction reaches 27-29PaS, in reactant, add aminosilane and carry out chemical reaction with pretreated polyether Glycols;
The 3rd step: dehydration is extracted
After above-mentioned reaction 10-15 hour, utilize vacuum pump that low molecular compound and water are deviate from, residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
Modified silicone rubber provided by the present invention and preparation method thereof is compared with prior art, have the following advantages: one, because the reaction of preparation modified silicone rubber is a kind of combination reaction, preparation technology's temperature is between 90-125 ℃, control easily, so this preparation technology has advantage of simple technology; Its two, can construct in a humid environment by the silicone sealant that this modified silicone rubber is prepared; Its three, less demanding when using the silicone sealant of modified silicone rubber preparation to make tackiness agent to the degree of cleaning of interface, need not special cleaning is made at the interface, therefore have the advantage of easy construction.
Embodiment
Embodiment 1:
The first step: to the processing of polyether Glycols
The polyether Glycols that takes by weighing 10 weight parts is inserted in the reactor, is evacuated to 300mmHg and is heated to 120 ℃ simultaneously, is incubated venting after 4 hours;
Second step: reaction
Isocyanic ester-the tolylene diisocyanate (TDI) that takes by weighing 1 weight part adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 50 hours, after the viscosity of resultant of reaction reaches 28PaS during after testing at 25 ℃, in reactant, add γ-An Bingjisanjiayangjiguiwan and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 10 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
Embodiment 2:
The polyether Glycols that takes by weighing 11 weight parts is inserted in the reactor, is evacuated to 250mmHg and is heated to 100 ℃ simultaneously, is incubated venting after 5 hours;
Second step: reaction
Taking by weighing the isocyanic ester of 2 weight parts---'-diphenylmethane diisocyanate (MDI) adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 40 hours, after the viscosity of resultant of reaction reaches 28PaS during after testing at 25 ℃, in reactant, add γ-aminopropyl methyldiethoxysilane and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 12 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
Embodiment 3:
The polyether Glycols that takes by weighing 12 weight parts is inserted in the reactor, is evacuated to 220mmHg and is heated to 95 ℃ simultaneously, is incubated venting after 8 hours;
Second step: reaction
Isocyanic ester-the hexamethylene diisocyanate (HDI) that takes by weighing 2.5 weight parts adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 30 hours, after the viscosity of resultant of reaction reaches 26PaS during after testing at 25 ℃, in reactant, add β-aminoethyl-γ-aminopropyl methyl dimethoxysilane and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 15 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
Embodiment 4:
The polyether Glycols that takes by weighing 9 weight parts is inserted in the reactor, is evacuated to 270mmHg and is heated to 110 ℃ simultaneously, is incubated venting after 6 hours;
Second step: reaction
Isocyanic ester-the isophorone diisocyanate (IPDI) that takes by weighing 1.5 weight parts adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 35 hours, after the viscosity of resultant of reaction reaches 29PaS during after testing at 25 ℃, in reactant, add N-(normal-butyl)-γ-An Bingjisanjiayangjiguiwan and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 11 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
Embodiment 5:
The polyether Glycols that takes by weighing 8 weight parts is inserted in the reactor, is evacuated to 200mmHg and is heated to 125 ℃ simultaneously, is incubated venting after 7 hours;
Second step: reaction
Isocyanic ester-the dicyclohexyl methane diisocyanate (HMDI) that takes by weighing 2 weight parts adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 45 hours, after the viscosity of resultant of reaction reaches 28PaS during after testing at 25 ℃, in reactant, add β-aminoethyl-γ-An Bingjisanjiayangjiguiwan and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 13 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
Embodiment 6:
The polyether Glycols that takes by weighing 10 weight parts is inserted in the reactor, is evacuated to 300mmHg and is heated to 90 ℃ simultaneously, is incubated venting after 6.5 hours;
Second step: reaction
Isocyanic ester-the xylylene diisocyanate (XDI) that takes by weighing 2.5 weight parts adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 40 hours, after the viscosity of resultant of reaction reaches 27PaS during after testing at 25 ℃, in reactant, add γ-An Bingjisanyiyangjiguiwan and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilized vacuum pump that low molecular compound and water are deviate from after 14 hours, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
With the silicone sealant of this product preparation, every after tested physical and chemical index is as follows
Interface need not use primary coat liquid and moist but do not have under the open fire situation and also can construct at interface during construction, and construction back adhesive effect is constant.
More than the sample that adopted of the detection data of each embodiment all are modified silicone rubbers of getting 3 prepared weight parts of each embodiment, the paraffin that adds 5 weight parts is therein done the silicon mountain range soil of softening agent, 2 weight parts and is done the A component that forms after the strengthening agent mixing and stirring, and do B component that the silicon mountain range soil mixing and stirring of the carbon black of paraffin, 1 weight part of catalyzer, 4 weight parts and 4 weight parts constitutes by A: B=1 with the dibutyltin diacetate of 1 weight part again: 1 weight proportion uses the detection data of the silicone sealant that constitutes.
After testing; modified silicone rubber via nitrogen protection can be preserved more than 3 years, and pressed A with the B component thus: B=1: 1 weight proportion uses the performance perameter of the silicone sealant that constitutes to press A with the modified silicone rubber and the B component of newborn output: B=1: 1 weight proportion uses the performance perameter of the silicone sealant that constitutes basic identical.
Claims (2)
1. modified silicone rubber, it is characterized in that by
The aminosilane ingredient of the isocyanic ester of the polyether Glycols of 8-12 weight part, 1-3 weight part and 2-5 weight part constitutes.
2. the method steps of the described a kind of modified silicone rubber of preparation claim 1 is:
The first step: to the processing of polyether Glycols
Take by weighing polyether Glycols and insert in the reactor, be evacuated to 200-300mm Hg, and be heated to 90-125 ℃ simultaneously, be incubated venting after 4-8 hour;
Second step: reaction
Taking by weighing isocyanic ester in proportion adds in the aforesaid reaction vessel, make it to carry out chemical reaction with pretreated polyether Glycols, and kept 30-50 hour, after the viscosity of resultant of reaction reaches 27-29PaS during at 25 ℃, in reactant, add aminosilane and carry out chemical reaction;
The 3rd step: dehydration is extracted
Above-mentioned reaction utilizes vacuum pump that low molecular compound and water are deviate from after carrying out 10-15 hour, and residuum is a modified silicone rubber;
The 4th step: packing
To charge into nitrogen protection in the modified silicone rubber that form.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100010093A CN101469067B (en) | 2008-03-25 | 2009-01-19 | Modified silicone rubber and preparation technique thereof |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100546956A CN101245145A (en) | 2008-03-25 | 2008-03-25 | Modified silicone rubber and preparation technique |
| CN200810054695.6 | 2008-03-25 | ||
| CN2009100010093A CN101469067B (en) | 2008-03-25 | 2009-01-19 | Modified silicone rubber and preparation technique thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101469067A CN101469067A (en) | 2009-07-01 |
| CN101469067B true CN101469067B (en) | 2011-06-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2008100546956A Pending CN101245145A (en) | 2008-03-25 | 2008-03-25 | Modified silicone rubber and preparation technique |
| CN2009100010093A Expired - Fee Related CN101469067B (en) | 2008-03-25 | 2009-01-19 | Modified silicone rubber and preparation technique thereof |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2008100546956A Pending CN101245145A (en) | 2008-03-25 | 2008-03-25 | Modified silicone rubber and preparation technique |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5851185B2 (en) * | 2010-10-29 | 2016-02-03 | 日清紡ブレーキ株式会社 | Friction material |
| CN102304282B (en) * | 2011-01-17 | 2013-01-09 | 海龙核材科技（江苏）有限公司 | Flame-retardant silicone rubber and preparation method thereof |
| CN105175685A (en) * | 2015-08-27 | 2015-12-23 | 江苏海龙核科技股份有限公司 | Modified silicone rubber and preparation process therefor |
| CN109439266A (en) * | 2018-08-20 | 2019-03-08 | 苏州市湘园特种精细化工有限公司 | A kind of preparation method of silane coupler modified still monocomponent polyurethane adhesive |
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2008
- 2008-03-25 CN CNA2008100546956A patent/CN101245145A/en active Pending
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- 2009-01-19 CN CN2009100010093A patent/CN101469067B/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN101469067A (en) | 2009-07-01 |
| CN101245145A (en) | 2008-08-20 |
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Inventor after: Zhang Guangqiang Inventor after: Chen Guanru Inventor before: Zhang Guangqiang |
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Free format text: CORRECT: INVENTOR; FROM: ZHANG GUANGQIANG TO: ZHANG GUANGQIANG CHEN GUANRU |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Hengshui Dazhong Rubber Plastic Co., Ltd. Assignor: Zhang Guangqiang Contract record no.: 2012130000019 Denomination of invention: Modified silicone rubber and preparation technique Granted publication date: 20110615 License type: Exclusive License Open date: 20090701 Record date: 20120305 |
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Granted publication date: 20110615 Termination date: 20170119 |
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