CN103319903A - Double-component addition type room-temperature vulcanizing silicone rubber and preparation method thereof - Google Patents
Double-component addition type room-temperature vulcanizing silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to double-component addition type room-temperature vulcanizing silicone rubber and a preparation method thereof. The double-component room-temperature vulcanizing silicone rubber comprises a component A and a component B; the mass ratio of the component A to the component B is 1:1. The component A is composed of 40-70 parts of vinyl end-capped organopolysiloxane with the viscosity of 300-1000 mPa.s, 20-45 parts of 100-1000-mesh silica powder and 0.1-5 parts of platinum catalyst; the component B is composed of 40-70 parts of vinyl end-capped organopolysiloxane with the viscosity of 300-1000 mPa.s, 20-45 parts of 100-1000-mesh silica powder, 5-10 parts of hydrogen-containing polysiloxane with the hydrogen content of 0.1-1.2% and 0.1-5 parts of inhibitor. The prepared double-component addition type room-temperature vulcanizing silicone rubber has good flowability and adhesive; the silicone rubber disclosed by the invention has low colourless transparent viscosity and good flowability and adhesive and is applied to encapsulating materials of electronic components; the method is simple and easy to operate; the double-component addition type room-temperature vulcanizing silicone rubber has a certain industrial application value.
Description
Technical field
The invention belongs to organosilicon self cure joint sealant field, be specifically related to a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method.
Background technology
Add-on type liquid silicon rubber does not produce by product in cross-linking vulcanized process, shrinking percentage is minimum, the energy deep layer is solidified, the material thing corrosion to contacting, and is the concern material of electric industry first-selection.The level that physical and mechanical properties after the sulfuration of addition liquid silastic and electrical property can meet or exceed melting silicone rubber, and because can injection molding and compression molding, have advantages such as easy to process, production efficiency, cost is low, energy-conservation, so some traditional melting silicone rubber goods is substituted by liquid silastic.
In addition, along with the develop rapidly of electronic industry, the high performance of electronic devices and components has proposed more and more higher requirement to its Embedding Material.When organo-silicone rubber carries out embedding, do not emit low molecule, unstressed contraction, but deep layer vulcanization does not have any corrosion, and transparent silica gel becomes transparent elastomer after sulfuration, high-visible to components and parts packaged in the glue-line, can arrive the inside measuring sensor parameter one by one with acupuncture, be convenient to detect and reprocess.So organo-silicone rubber progressively becomes the main flow Embedding Material of electronic component.
Electronic component is constantly microminiaturized, and colleague's component element long period contact with moisture with water, is corroded easily, and in order to protect the normal use of electronic component performance, it is simple that needs prepare a kind of technology, and modest viscosity is convenient to the organic silicon potting adhesive of embedding.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of double component room temperature vulcanization silicon rubber and preparation method at above drawback, to satisfy the extensive requirement of silastic material.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of dual composition addition type room temperature vulcanized silicone rubber is characterized by, and by weight for 1:1 forms, its component is counted composed as follows by weight by A component and B component:
The A component:
Organopolysiloxane 40-70 part of ethenyl blocking
Silicon dioxide powder 20-45 part
Platinum catalyst 0.1-5 part
Its gross weight umber is 100 parts;
The B component:
Organopolysiloxane 40-70 part of ethenyl blocking
Silicon dioxide powder 20-45 part
Hydrogen containing siloxane 5-10 part
Inhibitor 0.1-5 part
Its gross weight umber is 100 parts;
The preparation method of above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber, its preparation method is as follows:
(1) preparation component A: in kneader, add organopolysiloxane, the silicon dioxide powder of ethenyl blocking earlier, stirred 2-4 hour under the room temperature; Be warming up to 160-170 ℃, stirred 2-4 hour under the vacuum condition, stop vacuum then, the polysiloxane dilution is continued to add in the cooling back; Add platinum catalyst more in proportion, stir, namely get the A component;
(2) preparation component B: in kneader, add organopolysiloxane, the silicon dioxide powder of ethenyl blocking earlier, stirred 2-4 hour under the room temperature; Be warming up to 160-170 ℃, stirred 2-4 hour under the vacuum condition, stop vacuum then, the polysiloxane dilution is continued to add in the cooling back; Add hydrogen containing siloxane, inhibitor more in proportion, stir, namely get the B component;
(3) be that 1:1 mixes with A component and the B component that makes by mass ratio, namely get described dual composition addition type room temperature vulcanized silicone rubber.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, the organopolysiloxane viscosity of described ethenyl blocking is 300-1000mPa.s, the mass percent content of vinyl is 1.0-2.0%.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, the preparation method of the organopolysiloxane of described ethenyl blocking is as follows: by weight 100 parts of octamethylcyclotetrasiloxanes and 0.1-3 part tetramethyl divinyl disiloxane are mixed, under the state that stirs, add 0.01-0.5 part catalyzer Tetramethylammonium hydroxide, be warming up to 120-140 ℃ of polymerization 2-6 hour, be warming up to 150-200 ℃ again, under 0.08-0.09MPa vacuum tightness, took off low molecule 6-10 hour, and can obtain after the cooling.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described silicon dioxide powder is aerosil or the precipitated silica after the silane coupling agent hydrophobic is handled.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described platinum catalyst is Platinic chloride tetramethyl divinyl disiloxane complex compound, wherein the content of platinum is 1000-5000ppm.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described hydrogen containing siloxane viscosity is 100-600mPa.s, hydrogen content is 0.1-1.2%.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described hydrogen containing siloxane preparation method is as follows: the octamethylcyclotetrasiloxane with 100 parts of containing hydrogen silicone oils and 25-150 part is added in the reactor by weight, add 15-30 part an acidic catalyst, stir, reaction is 2-10 hour under 40-80 degree centigrade temperature, stop to stir, cooling, washing can obtain after the filtration.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described inhibitor be in vinyl ring body or the acetylene alcohol any.
Above-mentioned a kind of dual composition addition type room temperature vulcanized silicone rubber and preparation method thereof, wherein, described silane coupling agent is any one or the mixture more than two kinds in dimethyldiethoxysilane, dimethyldimethoxysil,ne, dimethyl cyclosiloxane, the hexamethyldisilazane.
Beneficial effect of the present invention is: two component addition room temperature vulcanized silicone rubbers that the present invention makes have good flowability and cementability, and this method is simple, easy to operate, and certain industrial application value is arranged.
Embodiment
Below by specific embodiment the specific embodiment of the present invention is described in further detail.
Example one
A kind of dual composition addition type room temperature vulcanized silicone rubber, its preparation method is as follows:
(1) preparation component A:
1. the organopolysiloxane for preparing ethenyl blocking: by weight 100 parts of octamethylcyclotetrasiloxanes and 3 parts of tetramethyl divinyl disiloxanes are mixed, under the state that stirs, add 0.5 part of catalyzer Tetramethylammonium hydroxide, be warming up to 140 ℃ of polyase 13s hour, be warming up to 200 ℃ again, under 0.08MPa vacuum tightness, took off low molecule 10 hour, can obtain after the cooling, its viscosity is 800mPa.s, and the mass percent content of vinyl is 1.5%;
2. the organopolysiloxane and the 150Kg precipitated silica that add the ethenyl blocking of 150kg in the 500L kneader stir agglomerating back room temperature and continue to stir 2 hours; Be warming up to 160-170 ℃, stirred 3 hours under the vacuum 0.8MPa condition, stop vacuum then, the organopolysiloxane dilution of 75kg ethenyl blocking is continued to add in the cooling back; Add the platinum catalyst of 1.13kg again, stir, namely get the A component, wherein, platinum catalyst is Platinic chloride tetramethyl divinyl disiloxane complex compound, and the content of its platinum is 1000-5000ppm;
(2) preparation component B:
1. prepare hydrogen containing siloxane: the octamethylcyclotetrasiloxane with 100 parts of containing hydrogen silicone oils and 150 parts is added in the reactor by weight, add 30 parts of an acidic catalysts, stir, reaction is 6 hours under 80 degrees centigrade temperature, stops to stir cooling, washing, can obtain after the filtration, its viscosity is 600mPa.s, and hydrogen content is 1.1%;
2. the organopolysiloxane and the 150Kg precipitated silica that add the 150kg ethenyl blocking in the 500L kneader stir agglomerating back room temperature and continue to stir 2 hours; Be warming up to 160-170 ℃, stirred 3 hours under the vacuum 0.8MPa condition, stop vacuum then, the organopolysiloxane of 75Kg ethenyl blocking is continued to add in the cooling back; Add the 69Kg hydrogen content again and be 0.1% hydrogen containing siloxane and the vinyl ring body of 8.14Kg, stir, namely get component B;
(3) be that 1:1 mixes with A component and the B component that makes by mass ratio, namely get described dual composition addition type room temperature vulcanized silicone rubber.
The technical parameter of the silica gel of preparation is as follows:
| Test event | Performance |
| Viscosity (mPa.s) | 7000 |
| Surface drying time (h) | 3 |
| Set time (h) | 21 |
| Density (g/cm 3) | 1.138 |
| Hardness (Shao Shi) | 42 |
| Tensile strength (MPa) | 7.1 |
| Tearing strength (KN/m) | 12.5 |
| Elongation at break (%) | 360 |
Example two
A kind of dual composition addition type room temperature vulcanized silicone rubber, its preparation method is as follows:
(1) preparation component A:
1. the organopolysiloxane for preparing ethenyl blocking: by weight 100 parts of octamethylcyclotetrasiloxanes and 3 parts of tetramethyl divinyl disiloxanes are mixed, under the state that stirs, add 0.5 part of catalyzer Tetramethylammonium hydroxide, be warming up to 140 ℃ of polyase 13s hour, be warming up to 200 ℃ again, under 0.08MPa vacuum tightness, took off low molecule 10 hour, can obtain after the cooling, its viscosity is 800mPa.s, and the mass percent content of vinyl is 1.5%;
2. the vinyl polysiloxane and the 80Kg silicon-dioxide that add 106.7Kg in the 500L kneader stir agglomerating back room temperature and continue to stir 2 hours; Be warming up to 160-170 ℃, stirred 3 hours under the vacuum 0.8MPa condition, stop vacuum then, the organopolysiloxane dilution of 63.3kg ethenyl blocking is continued to add in the cooling back, adds the platinum catalyst of 0.75Kg again, stirs, namely get the A component, wherein, platinum catalyst is Platinic chloride tetramethyl divinyl disiloxane complex compound, and the content of its platinum is 1000-5000ppm;
(2) preparation component B:
1. prepare hydrogen containing siloxane: the octamethylcyclotetrasiloxane with 100 parts of containing hydrogen silicone oils and 150 parts is added in the reactor by weight, add 30 parts of an acidic catalysts, stir, reaction is 6 hours under 80 degrees centigrade temperature, stops to stir cooling, washing, can obtain after the filtration, its viscosity is 600mPa.s, and hydrogen content is 1.1%;
2. the vinyl polysiloxane and the 80Kg silicon-dioxide that add 106.7Kg in the 500L kneader stir agglomerating back room temperature and continue to stir 2 hours; Be warming up to 160-170 ℃, stirred 3 hours under the vacuum 0.8MPa condition, stop vacuum then, the organopolysiloxane of 63.3Kg ethenyl blocking is continued to add in the cooling back; Add the 8.6Kg hydrogen content again and be 0.75% hydrogen containing siloxane and the acetylene alcohol of 4.74Kg, stir, namely get component B;
(3) be that 1:1 mixes with A component and the B component that makes by mass ratio, namely get described dual composition addition type room temperature vulcanized silicone rubber.
The technical parameter of the silica gel of preparation is as follows:
| Test event | Performance |
| Viscosity (mPa.s) | 6200 |
| Surface drying time (h) | 3 |
| Set time (h) | 21 |
| Density (g/cm 3) | 1.138 |
| Hardness (Shao Shi) | 47 |
| Tensile strength (MPa) | 7.9 |
| Tearing strength (KN/m) | 18 |
| Elongation at break (%) | 420 |
Here description of the invention and application is illustrative, is not to want that therefore, the present invention is not subjected to the restriction of present embodiment with scope restriction of the present invention in the above-described embodiments, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (10)
1. a dual composition addition type room temperature vulcanized silicone rubber is characterized by, and by weight for 1:1 forms, its component is counted composed as follows by weight by A component and B component:
The A component:
Organopolysiloxane 40-70 part of ethenyl blocking
Silicon dioxide powder 20-45 part
Platinum catalyst 0.1-5 part
Its gross weight umber is 100 parts;
The B component:
Organopolysiloxane 40-70 part of ethenyl blocking
Silicon dioxide powder 20-45 part
Hydrogen containing siloxane 5-10 part
Inhibitor 0.1-5 part
Its gross weight umber is 100 parts.
2. the preparation method of a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 is characterized by, and its preparation method is as follows:
(1) preparation component A: in kneader, add organopolysiloxane, the silicon dioxide powder of ethenyl blocking earlier, stirred 2-4 hour under the room temperature; Be warming up to 160-170 ℃, stirred 2-4 hour under the vacuum condition, stop vacuum then, the polysiloxane dilution is continued to add in the cooling back; Add platinum catalyst more in proportion, stir, namely get the A component;
(2) preparation component B: in kneader, add organopolysiloxane, the silicon dioxide powder of ethenyl blocking earlier, stirred 2-4 hour under the room temperature; Be warming up to 160-170 ℃, stirred 2-4 hour under the vacuum condition, stop vacuum then, the polysiloxane dilution is continued to add in the cooling back; Add hydrogen containing siloxane, inhibitor more in proportion, stir, namely get the B component;
(3) be that 1:1 mixes with A component and the B component that makes by mass ratio, namely get described dual composition addition type room temperature vulcanized silicone rubber.
3. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof is characterized by, and the organopolysiloxane viscosity of described ethenyl blocking is 300-1000mPa.s, and the mass percent content of vinyl is 1.0-2.0%.
4. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof, it is characterized by, the preparation method of the organopolysiloxane of described ethenyl blocking is as follows: by weight 100 parts of octamethylcyclotetrasiloxanes and 0.1-3 part tetramethyl divinyl disiloxane are mixed, under the state that stirs, add 0.01-0.5 part catalyzer Tetramethylammonium hydroxide, be warming up to 120-140 ℃ of polymerization 2-6 hour, be warming up to 150-200 ℃ again, under 0.08-0.09MPa vacuum tightness, took off low molecule 6-10 hour, and can obtain after the cooling.
5. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof is characterized by, and described silicon dioxide powder is aerosil or the precipitated silica after the silane coupling agent hydrophobic is handled.
6. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof is characterized by, and described platinum catalyst is Platinic chloride tetramethyl divinyl disiloxane complex compound, and wherein the content of platinum is 1000-5000ppm.
7. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof is characterized by, and described hydrogen containing siloxane viscosity is 100-600mPa.s, and hydrogen content is 0.1-1.2%.
8. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof, it is characterized by, described hydrogen containing siloxane preparation method is as follows: the octamethylcyclotetrasiloxane with 100 parts of containing hydrogen silicone oils and 25-150 part is added in the reactor by weight, add 15-30 part an acidic catalyst, stir, reaction is 2-10 hour under 40-80 degree centigrade temperature, stop to stir, cooling, washing can obtain after the filtration.
9. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof is characterized by, described inhibitor be in vinyl ring body or the acetylene alcohol any.
10. a kind of dual composition addition type room temperature vulcanized silicone rubber as claimed in claim 1 or 2 and preparation method thereof, it is characterized by, described silane coupling agent is any one or the mixture more than two kinds in dimethyldiethoxysilane, dimethyldimethoxysil,ne, dimethyl cyclosiloxane, the hexamethyldisilazane.
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| CN104650598A (en) * | 2014-03-13 | 2015-05-27 | 冯德平 | Two-component organosilicone plasticine |
| CN105111750A (en) * | 2015-09-09 | 2015-12-02 | 蓝星（成都）新材料有限公司 | Organosilicon sealant for LED (light-emitting diode) packaging |
| CN105367798A (en) * | 2015-11-27 | 2016-03-02 | 广州市银讯光电科技有限公司 | Organic silicon base adhesive for packaging LED chip and preparation method thereof |
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| CN104650598A (en) * | 2014-03-13 | 2015-05-27 | 冯德平 | Two-component organosilicone plasticine |
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| CN105968819A (en) * | 2016-05-12 | 2016-09-28 | 浙江新安化工集团股份有限公司 | Key liquid silicone rubber composition with ultralong striking life and preparation method of key liquid silicone rubber composition |
| CN106751891A (en) * | 2016-12-02 | 2017-05-31 | 镇江高美新材料有限公司 | A kind of anti-oxidant high-temperature resisting liquid silicon rubber and preparation method thereof |
| CN110294934A (en) * | 2018-03-23 | 2019-10-01 | 英济股份有限公司 | Liquid-state silastic compositions and its manufacturing method and oral cavity isolator |
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| CN108822723A (en) * | 2018-05-31 | 2018-11-16 | 镇江高美新材料有限公司 | A kind of liquid silicon rubber composition of engineering plastic modification |
| CN111057520A (en) * | 2019-12-31 | 2020-04-24 | 兆舜科技(广东)有限公司 | Double-component addition type pouring sealant and preparation method and application thereof |
| CN111057520B (en) * | 2019-12-31 | 2021-10-22 | 兆舜科技(广东)有限公司 | Double-component addition type pouring sealant and preparation method and application thereof |
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