CN103408941A - Transparent dealcoholized single-component room temperature vulcanized silicone rubber and preparation method thereof - Google Patents
Transparent dealcoholized single-component room temperature vulcanized silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses transparent dealcoholized single-component room temperature vulcanized silicone rubber and a preparation method thereof. The rubber is prepared from the following raw materials in percentage by weight: 75-90% of alpha-omega-dihydroxyl polydimethylsiloxane, 1-5% of an end-capping reagent, 0.1-2% of hydroxyl remover, 0.1-2% of end-capping catalyst, 1-15% of white carbon black reinforcing filler, 1-6% of siloxane compound crosslinking agent, 0.01-2% of siloxane titanate ester catalyst, 0.01-2% of organic tin catalyst, 0.01-3% of silane coupling agent and 1-10% of alkane mixture plasticizer. According to the rubber disclosed by the invention, the novel end-capping reagent and the novel end-capping catalyst are used, so that the semi-product is stable in physical property and beneficial to storage. When product rubber is produced, the reaction is stable to prevent gelation. The titanate catalyst is used for effectively preventing yellowing of the sizing material, so that the storage stability of the product is improved.
Description
Technical field
The present invention relates to a kind of transparent dealcoholized single-component room temperature vulcanized silicone rubber, also relate to a kind of preparation method of transparent dealcoholized single-component room temperature vulcanized silicone rubber.
Background technology
Dealcoholized silicone rubber is each major company's most study of the eighties world, description and quantity type with fastest developing speed, new achievement in research makes this system that very much progress arranged aspect vulcanization rate, stability in storage, cohesiveness and flame retardant resistance, its range of application is enlarged rapidly, become principal item and the developing direction of room temperature vulcanized silicone rubber.The variegated glue of dealcoholysis in recent years has a great development, but the product of the transparent class of pure type does not have progress always.The performance of alcohol type transparent adhesive tape is compared and is had the following advantages with other transparent series products: (1), have an excellent transmittance; (2), the electrical insulation capability excellence, moistureproof, anticorona; (3), has good high and low temperature resistance; (4), yellowing resistance can be good; (5), due to the volatile gas of dealcoholysis class, not to two-way mirror, brass, the material corrosion infiltration such as zinc-plated, widely applicable, have a feature of environmental protection.
There are this relatively ripe series products in current German Wa Ke company, Dow corning company, but by the each side test, find all to exist the defect of some aspect of performances.The research of domestic this series products and production still are in the exploratory stage, and the defect existed is larger.
When in prior art, Dealcoholized One part Room Temperature Vulcanized Silicone Rubber is produced, because of α, silicon hydroxyl in alpha, omega-dihydroxy polydimethyl siloxane easily and catalyzer organotin, titanium complex generation condensation reaction, make rapid increase, viscosity increased in the polymkeric substance molar mass short period of time, simultaneously the silicon alkyl easily and the alkyl generation hydrogen bond association of inorganic filler surface, cause the phenomenon that can't add and disperse, thereby make blend glue stuff cause the structurizing phenomenon to lose processing characteristics.In prior art multiplex titanium complex is as catalyzer, and the easy like this sizing material flavescence phenomenon that causes.
Summary of the invention
Technical problem to be solved by this invention is to provide on a kind of basis keeping end properties and prevents the sizing material xanthochromia, the work in-process storage time is fixed on to a kind of transparent dealcoholized single-component room temperature vulcanized silicone rubber in OK range.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of transparent dealcoholized single-component room temperature vulcanized silicone rubber, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 75～90%, end-capping reagent 1～5%, hydroxyl removes agent 0.1～2%, end-blocking catalyzer 0.1～2%, white carbon black reinforced filling 1～15%, silicone compounds linking agent 1～6%, metatitanic acid silicone esters catalyzer 0.01～2%, organic tin catalyzer 0.01～2%, silane coupling agent 0.01～3%, paraffins mixture softening agent 1～10%.
As preferred technical scheme, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 78%, end-capping reagent 1.6%, hydroxyl removes agent 0.6%, end-blocking catalyzer 0.2%, white carbon black reinforced filling 11%, silicone compounds linking agent 6%, metatitanic acid silicone esters catalyzer 0.1%, organic tin catalyzer 0.1%, silane coupling agent 0.2%, paraffins mixture softening agent 2.2%.
As to improvement of the technical scheme, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 83.5%, end-capping reagent 1.6%, hydroxyl removes agent 0.6%, end-blocking catalyzer 0.4%, white carbon black reinforced filling 9%, silicone compounds linking agent 3%, metatitanic acid silicone esters catalyzer 0.3%, organic tin catalyzer 0.06%, silane coupling agent 0.24%, paraffins mixture softening agent 1.3%.
As to further improvement in the technical proposal, described α, the molecular weight of alpha, omega-dihydroxy polydimethyl siloxane between 5000～12000g/mol, kinetic viscosity 10000～100000Pa.s;
Described end-capping reagent is polyfunctional group organoalkoxysilane series products;
Described white carbon black reinforced filling is the white carbon black of different specific surface areas;
Described metatitanic acid silicone esters catalyzer is reacted and makes with alkyl alcohol by isopropyl titanate;
Described organic tin catalyzer is dibutyl tin laurate;
Described silane coupling agent is the silane coupling agent that contains epoxy group(ing);
Described paraffins mixture softening agent is the mixture of paraffinic hydrocarbons, naphthenic hydrocarbon and aromatic hydrocarbon, is 1～20Pa.s under the kinetic viscosity room temperature of described paraffins mixture softening agent.
As the further improvement to technique scheme, it is at least a in silazane, aza-cyclopentane, piperidine, carbamate silane and epoxy radicals silicone hydride that described hydroxyl removes agent;
Described end-blocking catalyzer is at least a in alkali metal hydroxide, organic amine compound, phosphoric acid ester, the compound that contains oximido and Potassium ethanoate;
The general formula of described silicone compounds linking agent is R1nSi (OR2) 4-n, 1≤n≤4, and wherein R1 is the saturated or undersaturated alkyl of straight chain or side chain, in n >=2 o'clock, the alkyl of R1 representative is identical or not identical; In 4-n >=2 o'clock, R2 representative alkyl is identical or not identical.
Another technical problem to be solved by this invention is to provide a kind of preparation method of bright Dealcoholized one-component room temperature vulcanized silicone rubber.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation method of transparent dealcoholized single-component room temperature vulcanized silicone rubber, comprise the following steps:
The first step: by weight percentage by 75～90% α, the end-blocking catalyzer that alpha, omega-dihydroxy polydimethyl siloxane and 1～5% end-capping reagent, 0.1～2% hydroxyl remove agent and 0.1～2% joins in reactor the vacuum stirring for the first time of heating and carries out end capping; By the work in-process after end capping store 5～10 days stand-by;
Second step: work in-process are put into to whipping appts, carry out vacuum stirring for the second time after adding by weight percentage the paraffins mixture softening agent of 1～15% white carbon black reinforced filling and 1～10%;
The 3rd step: carry out vacuum stirring for the third time after the silane coupling agent that adds by weight percentage 1～6% silicone compounds linking agent, 0.01～2% metatitanic acid silicone esters catalyzer, 0.01～2% organic tin catalyzer and 0.01～3% in whipping appts;
The 4th step: carry out the discharging packing, obtain the finished product.
As preferred technical scheme, in the described the first step, the vacuum tightness of reactor is that to be controlled at 60～80 ℃, the stirrer rotating speed of reactor be that 28～35r/s stirs 60～180min for 0.09～0.12MPa, temperature, then be warming up to 120～130 ℃, insulation finds time to stir 180～200min;
In described second step, vacuum tightness is that 0.09～0.12MPa, stirrer rotating speed are that 45～55r/s stirs 40～50min;
In described the 3rd step, vacuum tightness is that 0.09～0.12MPa, stirrer rotating speed are that 36～46r/s stirs 30～40min.
As to improvement of the technical scheme, the described the first step for the first time vacuum tightness 0.09MPa, the temperature of vacuum stirring to be controlled at 60-80 ℃, stirrer rotating speed be that 28r/s stirs 60-180min, then be warming up to 120 ℃ of insulations and find time to stir 180min, after end-blocking, store a week rear stand-by;
In described second step for the second time the vacuum tightness of vacuum stirring be that 0.09MPa, stirrer rotating speed are that 45r/s stirs 40min;
In described the 3rd step for the third time the vacuum tightness of vacuum stirring be that 0.09MPa, stirrer rotating speed are that 36r/s stirs 30min.
As to improvement of the technical scheme, described α, the molecular weight of alpha, omega-dihydroxy polydimethyl siloxane between 5000～12000g/mol, kinetic viscosity 10000～100000Pa.s;
Described end-capping reagent is polyfunctional group organoalkoxysilane series products;
Described white carbon black reinforced filling is the white carbon black of different specific surface areas;
Described metatitanic acid silicone esters catalyzer is reacted and makes with alkyl alcohol by isopropyl titanate;
Described organic tin catalyzer is dibutyl tin laurate;
Described silane coupling agent is the silane coupling agent that contains epoxy group(ing);
Described paraffins mixture softening agent is the mixture of paraffinic hydrocarbons, naphthenic hydrocarbon and aromatic hydrocarbon, is 1～20Pa.s under the kinetic viscosity room temperature of described paraffins mixture softening agent.
As to further improvement in the technical proposal, it is at least a in silazane, aza-cyclopentane, piperidine, carbamate silane and epoxy radicals silicone hydride that described hydroxyl removes agent;
Described end-blocking catalyzer is at least a in alkali metal hydroxide, organic amine compound, phosphoric acid ester, the compound that contains oximido and Potassium ethanoate;
The general formula of described silicone compounds linking agent is R1nSi (OR2) 4-n, 1≤n≤4, and wherein R1 is the saturated or undersaturated alkyl of straight chain or side chain, in n >=2 o'clock, the alkyl of R1 representative is identical or not identical; In 4-n >=2 o'clock, R2 representative alkyl is identical or not identical.
Owing to having adopted technique scheme, in order to prevent the sizing material structurizing, adopted suitable end-capping reagent, and success obtains stable work in-process after end-blocking, viscosity can not play acute variation in process of production, and product shelf life is strengthened; In order to prevent the xanthochromia of sizing material, adopt the titanic acid ester compound, obtained good effect.The present invention has used novel end-capping reagent, makes the work in-process physical property stable, is conducive to store, and reacting balance when finished product glue is produced, prevent gel, used titanate catalyst, effectively prevents the xanthochromia of sizing material, improved the stability in storage of product.
Claims (10)
1. a transparent dealcoholized single-component room temperature vulcanized silicone rubber, is characterized in that, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 75～90%, end-capping reagent 1～5%, hydroxyl remove agent 0.1～2%, end-blocking catalyzer 0.1～2%, white carbon black reinforced filling 1～15%, silicone compounds linking agent 1～6%, metatitanic acid silicone esters catalyzer 0.01～2%, organic tin catalyzer 0.01～2%, silane coupling agent 0.01～3%, paraffins mixture softening agent 1～10%.
2. transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 1, is characterized in that, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 78%, end-capping reagent 1.6%, hydroxyl remove agent 0.6%, end-blocking catalyzer 0.2%, white carbon black reinforced filling 11%, silicone compounds linking agent 6%, metatitanic acid silicone esters catalyzer 0.1%, organic tin catalyzer 0.1%, silane coupling agent 0.2%, paraffins mixture softening agent 2.2%.
3. transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 1, is characterized in that, raw material is made by following weight percent: α, alpha, omega-dihydroxy polydimethyl siloxane 83.5%, end-capping reagent 1.6%, hydroxyl remove agent 0.6%, end-blocking catalyzer 0.4%, white carbon black reinforced filling 9%, silicone compounds linking agent 3%, metatitanic acid silicone esters catalyzer 0.3%, organic tin catalyzer 0.06%, silane coupling agent 0.24%, paraffins mixture softening agent 1.3%.
4. transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 1, is characterized in that, described α, the molecular weight of alpha, omega-dihydroxy polydimethyl siloxane between 5000～12000g/mol, kinetic viscosity 10000～100000Pa.s;
Described end-capping reagent is polyfunctional group organoalkoxysilane series products;
Described white carbon black reinforced filling is the white carbon black of different specific surface areas;
Described metatitanic acid silicone esters catalyzer is reacted and makes with alkyl alcohol by isopropyl titanate;
Described organic tin catalyzer is dibutyl tin laurate;
Described silane coupling agent is the silane coupling agent that contains epoxy group(ing);
Described paraffins mixture softening agent is the mixture of paraffinic hydrocarbons, naphthenic hydrocarbon and aromatic hydrocarbon, is 1～20Pa.s under the kinetic viscosity room temperature of described paraffins mixture softening agent.
5. as claim 1,2,3 or 4 described transparent dealcoholized single-component room temperature vulcanized silicone rubbers, it is characterized in that, it is at least a in silazane, aza-cyclopentane, piperidine, carbamate silane and epoxy radicals silicone hydride that described hydroxyl removes agent;
Described end-blocking catalyzer is at least a in alkali metal hydroxide, organic amine compound, phosphoric acid ester, the compound that contains oximido and Potassium ethanoate;
The general formula of described silicone compounds linking agent is R1nSi (OR2) 4-n, 1≤n≤4, and wherein R1 is the saturated or undersaturated alkyl of straight chain or side chain, in n >=2 o'clock, the alkyl of R1 representative is identical or not identical; In 4-n >=2 o'clock, R2 representative alkyl is identical or not identical.
6. the preparation method of a transparent dealcoholized single-component room temperature vulcanized silicone rubber, is characterized in that, comprises the following steps:
The first step: by weight percentage by 75～90% α, the end-blocking catalyzer that alpha, omega-dihydroxy polydimethyl siloxane and 1～5% end-capping reagent, 0.1～2% hydroxyl remove agent and 0.1～2% joins in reactor the vacuum stirring for the first time of heating and carries out end capping; By the work in-process after end capping store 5～10 days stand-by;
Second step: work in-process are put into to whipping appts, carry out vacuum stirring for the second time after adding by weight percentage the paraffins mixture softening agent of 1～15% white carbon black reinforced filling and 1～10%;
The 3rd step: carry out vacuum stirring for the third time after the silane coupling agent that adds by weight percentage 1～6% silicone compounds linking agent, 0.01～2% metatitanic acid silicone esters catalyzer, 0.01～2% organic tin catalyzer and 0.01～3% in whipping appts;
The 4th step: carry out the discharging packing, obtain the finished product.
7. the preparation method of transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 6, is characterized in that,
In the described the first step vacuum tightness of reactor be 0.09～0.12MPa, temperature to be controlled at 60～80 ℃, the stirrer rotating speed of reactor be that 28～35r/s stirs 60～180min, then be warming up to 120～130 ℃, insulation finds time to stir 180～200min;
In described second step, vacuum tightness is that 0.09～0.12MPa, stirrer rotating speed are that 45～55r/s stirs 40～50min;
In described the 3rd step, vacuum tightness is that 0.09～0.12MPa, stirrer rotating speed are that 36～46r/s stirs 30～40min.
8. the preparation method of transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 7, is characterized in that,
The described the first step for the first time vacuum tightness 0.09MPa, the temperature of vacuum stirring to be controlled at 60-80 ℃, stirrer rotating speed be that 28r/s stirs 60-180min, then be warming up to 120 ℃ of insulations and find time to stir 180min, after end-blocking, store after a week stand-by;
In described second step for the second time the vacuum tightness of vacuum stirring be that 0.09MPa, stirrer rotating speed are that 45r/s stirs 40min;
In described the 3rd step for the third time the vacuum tightness of vacuum stirring be that 0.09MPa, stirrer rotating speed are that 36r/s stirs 30min.
9. the preparation method of transparent dealcoholized single-component room temperature vulcanized silicone rubber as claimed in claim 6, is characterized in that, described α, the molecular weight of alpha, omega-dihydroxy polydimethyl siloxane between 5000～12000g/mol, kinetic viscosity 10000～100000Pa.s;
Described end-capping reagent is polyfunctional group organoalkoxysilane series products;
Described white carbon black reinforced filling is the white carbon black of different specific surface areas;
Described metatitanic acid silicone esters catalyzer is reacted and makes with alkyl alcohol by isopropyl titanate;
Described organic tin catalyzer is dibutyl tin laurate;
Described silane coupling agent is the silane coupling agent that contains epoxy group(ing);
Described paraffins mixture softening agent is the mixture of paraffinic hydrocarbons, naphthenic hydrocarbon and aromatic hydrocarbon, is 1～20Pa.s under the kinetic viscosity room temperature of described paraffins mixture softening agent.
10. as the preparation method of claim 6,7,8 or 9 described transparent dealcoholized single-component room temperature vulcanized silicone rubbers, it is characterized in that, it is at least a in silazane, aza-cyclopentane, piperidine, carbamate silane and epoxy radicals silicone hydride that described hydroxyl removes agent;
Described end-blocking catalyzer is at least a in alkali metal hydroxide, organic amine compound, phosphoric acid ester, the compound that contains oximido and Potassium ethanoate;
The general formula of described silicone compounds linking agent is R1nSi (OR2) 4-n, 1≤n≤4, and wherein R1 is the saturated or undersaturated alkyl of straight chain or side chain, in n >=2 o'clock, the alkyl of R1 representative is identical or not identical; In 4-n >=2 o'clock, R2 representative alkyl is identical or not identical.
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| CN104059361A (en) * | 2014-06-09 | 2014-09-24 | 蓝星（成都）新材料有限公司 | Room-temperature quick-curing silicon rubber and preparation method thereof |
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Application publication date: 20131127 |