CN103160130A - Organic silicon thermoplastic elastomer and preparation method for same - Google Patents
Organic silicon thermoplastic elastomer and preparation method for same Download PDFInfo
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- CN103160130A CN103160130A CN2013101219083A CN201310121908A CN103160130A CN 103160130 A CN103160130 A CN 103160130A CN 2013101219083 A CN2013101219083 A CN 2013101219083A CN 201310121908 A CN201310121908 A CN 201310121908A CN 103160130 A CN103160130 A CN 103160130A
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Abstract
The invention discloses an organic silicon thermoplastic elastomer material and a preparation method for the same. The organic silicon thermoplastic elastomer material is characterized in that a thermoplastic elastomer is composed of organic silicon rubber, organic silicon resin and a crosslinking system; and the thermoplastic elastomer is prepared according to the following process steps of: preparing the thermoplastic elastomer by enabling the organic silicon rubber, the organic silicon resin and the crosslinking system to achieve intermolecular blending in solution, or uniformly mixing the organic silicon rubber, the organic silicon resin and the crosslinking system via a kneader or a double-screw extruder in a temperature condition of greater than 100 DEG C, and then preparing the high-performance dynamically-vulcanized organic silicon thermoplastic elastomer. Compared with other thermoplastic elastomers, the material is more capable of exerting the high-temperature resistance and ultraviolet resistance of organic silicon materials, excellent in optical transmission, and capable of being widely applied to the fields of solar energy, buildings, automobiles and medical treatment.
Description
Technical field:
The present invention relates to a kind of organosilicon thermoplastic elastic material and preparation method thereof, belong to organosilicon macromolecule material preparation field.
Technical background:
Thermoplastic elastomer has the use properties of elastic caoutchouc and the processing characteristics of plastics concurrently, can repeatedly repeat processing, has economic worth in following Materials.Current, widely used thermoplastic elastic material comprises polystyrene type, polyolefins and polyurethanes.Organosilicon material is used for all conglomeraties such as building, electronics, water treatment, space flight and the energy due to abilities such as having excellent weathering resistance, high-low temperature resistant.Existing organosilicon material adopts room temperature or hot crosslinked method once shaped usually, cannot repeat processing, thereby the organosilicon thermoplastic elastic material extensively receives publicity due to easy molding mode and good use properties.
1970, John C S, David J G and Sarah Lindsey publish an article in " Macromolecules " magazine the 3rd volume " Block Copolymers of polydimethylsiloxane and Polystyrene " progressively cause styrene monomer and hexamethyl cyclotrisiloxane monomer generation active anionic polymerization by n-Butyl Lithium, prepare the two component segmented copolymers of polysiloxane-polystyrene, molecular weight is usually 10
5Below g/mol, whole polymerization process is carried out under the anhydrous and oxygen-free condition, severe reaction conditions.
calendar year 2001, Brown D A and Price G J publish an article on " Polymer " magazine the 42 volume " Preparation and thermal properties of block copolymer of PDMS with styrene and methyl methacrylate usingATRP ", contain organo-siloxane segment macromole evocating agent by preparation and then further cause the active free radical polymerization of vinylbenzene or methacrylic acid monomer, prepare the thermoplastic elastic material that contains the organosilicon segment, the method need to prepare in advance macromole evocating agent and control the efficiency of initiation of initiator, the thermoplastic elastomer for preparing is worth segment by organosilicon segment and vinylbenzene or methacrylic acid and jointly forms.
US 6362287 discloses a kind of method of using the standby thermoplastic elastomer of Organosiliconpolymermodified modified nylon, adopts Dynamic Thermal sulfuration legal system for obtaining the thermoplastic elastic material that massfraction 35%-85% is nylon in preparation process at least under the condition of 210 ℃ by twin screw extruder.Similarly, US 6479580, US6649704, US20060229417 disclose respectively and have used Organosiliconpolymermodified modified polyolefine, polymeric amide and polyphenyl thioether material, and preparing the chief component that can repeat to process is the method for the thermoplastic elastic material of polyolefine, polyamine and polyphenylene sulfide.CN 102153853A discloses a kind of thermoplastic elastic material that uses polyurethane/silicon rubber and preparation method thereof.In the prepared material of above-mentioned method, organosilicon material is one of composition of the final thermoplastic material that forms just, can not bring into play in the use the resistance toheat of organosilicon material fully, resistance to elevated temperatures.In case and prepare at present just not reproducible processing after silicone elastomer material cross moulding, the polymkeric substance that can reuse forms entirely and yet there are no relevant report for the thermoplastic elastomer of organosilicon material.
Summary of the invention
The objective of the invention is provides a kind of organosilicon thermoplastic elastomer and preparation method thereof for the deficiencies in the prior art, is characterized in the full organosilicon polymer that consists of of organosilicon thermoplastic elastomer polymer that preparation method of the present invention prepares; Have certain second-order transition temperature, can repeat machine-shaping.
Purpose of the present invention realizes by following technical measures, and wherein said raw material umber is parts by weight except specified otherwise.
The starting raw material of organosilicon thermoplastic elastomer is composed of the following components:
100 parts of organo-silicone rubbers
Silicone resin 50-2000 part
Cross-linking system 0.08-30 part.
Organo-silicone rubber is the organopolysiloxane of linearity or branching, its chemical structural formula:
(R
1 3SiO
1/2)
x(R
2 2SiO
2/2)
y(R
3SiO
3/2)
z
Wherein, x and y are 1 to 1000 positive integers, and z is 0 or 1 to 1000 positive integer;
R
1, R
2And R
3Be hydrogen, amino, phenyl, C
1-20Alkyl, C
1-20Alkyl phenyl, C
1-20Alkoxyl group or contain C
2-8Identical or different organic group in thiazolinyl.
The abovementioned alkyl group is preferably from methyl, ethyl, propyl group, sec.-propyl, normal-butyl, the tertiary butyl, more preferably in methyl, ethyl, propyl group;
The above-mentioned organic group that contains thiazolinyl is selected from vinyl, allyl group, propenyl, butenyl, pentenyl, hexenyl, heptenyl, octenyl, norbornylene and tetrahydrobenzene, more preferably vinyl, allyl group;
The chemical structural formula of silicone resin is:
R
4 3SiO
1/2Unit and SiO
4/2Unit MQ resin, or contain R
5SiO
3/2Unit and R
6 2SiO
2/2The TD resin of unit, or contain R
4 3SiO
1/2Unit and R
5SiO
3/2The MT resin of unit, or contain R
4 3SiO
1/2Unit, R
5SiO
3/2Unit and R
6 2SiO
2/2At least a in the MTD resin of unit; M wherein, D, T, Q are term commonly used in the organosilicon industry, represent respectively simple function, two senses, trifunctional, four sense link units.
R wherein
4, R
5And R
6Be hydrogen, amino, phenyl, C
1-20Alkyl, C
1-20Alkyl phenyl, C
1-20Alkoxyl group or contain C
2-8Identical or different organic group in thiazolinyl;
The abovementioned alkyl group is selected from methyl, ethyl, propyl group, sec.-propyl, normal-butyl, the tertiary butyl, more preferably in methyl, ethyl, propyl group;
The above-mentioned organic group that contains thiazolinyl is selected from vinyl, allyl group, propenyl, butenyl, pentenyl, hexenyl, heptenyl, octenyl, norbornylene and tetrahydrobenzene, more preferably vinyl, allyl group;
In the mixture that described organo-silicone rubber and silicone resin form, need comprise at least 2 organic groups that contain thiazolinyl;
The described organic group that contains thiazolinyl can be provided or be provided or by both jointly providing by silicone resin by organo-silicone rubber, the organic group and the organo-silicone rubber mass ratio that contain thiazolinyl are 0.0005 ~ 0.20: 1, be preferable over 0.0008 ~ 0.20: 1, more preferably in 0.001 ~ 0.15: 1;
Described cross-linking system is organo-peroxide or/and at least a or two in organic hydrogen polysiloxanes;
Described organo-peroxide is 1,1
"-two (t-butyl peroxy) 3,3,5-trimethyl-cyclohexane, 2,5-dimethyl-2,5 two (t-butyl peroxy) hexane, 2,5-dimethyl-2, at least a in 5-two (t-butyl peroxy) acetylene.
Described organic hydrogen polysiloxanes is for containing at least the organopolysiloxane of two silicon-hydrogen bonds.
Also can comprise catalyzer in described cross-linking system, described catalyzer is that the complex compound, four (triphenylphosphine) of Platinic chloride or Platinic chloride and vinylsiloxane closes at least a in palladium and three (triphenylphosphine) rhodium chloride; Wherein, catalyzer: the quality ratio of organo-silicone rubber is 0 ~ 0.03: 1, is preferable over: 0 ~ 0.02: 1, if add urge body agent quality on the low side, the elastic properties of materials for preparing is not enough, and the higher meeting of catalyst system quality that adds causes material cost greatly to increase.
In order to make the organosilicon thermoplastic elastic material for preparing have better mechanical property, ageing resistance, flame retardant properties and processing characteristics etc., can also (for example add corresponding reinforcement, toughness reinforcing filler in this elastomer material, carbon black, silicon-dioxide etc.), antiaging agent (as sterically hindered phenol), fire retardant (as nitrogen, phosphine compound) and fluidizer etc., add-on depending on the material applications of relevant auxiliary agent.
Described organosilicon process for preparation of thermoplastic elastomer comprises the following steps:
(1) 100 parts of organo-silicone rubbers, 2000 parts of silicone resin 50-, cross-linking system 0.08-30 part are mixed in solvent or mixing machine;
(2) mix 2 – 300 minutes 20-250 ℃ of temperature, obtain 150 ℃ of second-order transition temperature 70 – of organic thermoplastic elastic;
Wherein organic solvent is at least a in toluene, dimethylbenzene, tetrahydrofuran (THF), methylene dichloride.
Performance test:
1, the molecular weight of organo-silicone rubber and silicone resin is measured by gel permeation chromatograph (GPC) under 25 ℃ of conditions, take the polystyrene molecular weight as standard;
2, tensile strength and elongation at break are with reference to GB/T 528-2009 standard test;
3, softening temperature is measured by ring and ball method.
The present invention has following advantage
1, by the preparation-obtained organosilicon thermoplastic elastomer of the present invention, its polymer architecture is entirely organosilicon polymer, can give full play to the performance advantages such as heat-resisting, cold-resistant, weather-proof, the anti-ozone of organosilicon polymer material, ventilative, biologically inert;
2, this elastomerics can also inject, extrude, the moulding such as mold pressing, but reprocessabilty, material can be used as building adhesive glue, LED immobilization material, solar panel encapsulation with numerous areas such as material, coating adhesive, pressure sensitive adhesives;
3, preparation technology is simple, and is efficient, easily amplifies and carry out suitability for industrialized production.
Embodiment
Below by embodiment, the present invention is specifically described, be necessary to be pointed out that at this present embodiment only is used for the present invention is further illustrated, but can not be interpreted as limiting the scope of the invention.The person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Under 25 ℃ of conditions, the methyl silicone rubber that 50 grams is contained vinyl is dissolved in 250 milliliters of toluene and methylene dichloride mixing solutions, MQ resin 100 grams that add again molecular weight 5500, add hydrogen containing siloxane 0.15 gram and Platinic chloride 0.05 gram after mixing, the mass ratio of therein ethylene base and organo-silicone rubber is 0.011: 1.Be warming up to 80 ℃ of reactions 50 minutes after adding catalyst system, then decompression is heated up in a steamer desolvation and is prepared the organosilicon thermoplastic elastomer, 84 ℃ of products therefrom softening temperatures, tensile strength 2.18 MPa, elongation at break 314%.
Embodiment 2
Under 25 ℃ of conditions, the methyl silicone rubber that 50 grams is contained vinyl is dissolved in the mixing of 250 milliliters of toluene and tetrahydrofuran (THF), TD resin 120 grams that contain vinyl that add again molecular weight 8500, add after mixing and contain 1, two (t-butyl peroxy) 3 of 1-, 3,5-trimethyl-cyclohexane, 0.3 gram, therein ethylene base and organo-silicone rubber mass ratio are 0.002: 1.Stir desolvation after 30 minutes after adding superoxide, then be warming up to 150
oC reaction 30 minutes prepares the organosilicon thermoplastic elastomer, 90 ℃ of products therefrom softening temperatures, tensile strength 3.11MPa, elongation at break 216%.
Embodiment 3
Under 25 ℃ of conditions, 20 grams are contained the methyl silicone rubber of vinyl and the phenyl siloxane rubber of 20 grams is dissolved in the mixing of 250 milliliters of tetrahydrofuran (THF)s, MQ resin 120 grams that contain vinyl that add again molecular weight 11500, TD silicone resin 30 grams of molecular weight 9000, add after mixing and contain two (t-butyl peroxy) 3,3 of 1,1-, 5-trimethyl-cyclohexane 0.8 gram, therein ethylene base and organo-silicone rubber mass ratio are 0.012: 1.Stir desolvation after 30 minutes after adding superoxide, then be warming up to 150
oC reaction 10 minutes prepares the organosilicon thermoplastic elastomer, 90 ℃ of products therefrom softening temperatures, tensile strength 3.41 MPa, elongation at break 200%.
Embodiment 4
Under 25 ℃ of conditions, 20 grams are contained the phenyl of the methyl of vinyl/ethyl silicon rubber and 20 grams/propyl group silicon rubber to be dissolved in the mixing of 250 milliliters of toluene and tetrahydrofuran (THF), MQ resin 20 grams that contain vinyl that add again molecular weight 11500, TD silicone resin 20 grams of molecular weight 9000, add after mixing and contain two (t-butyl peroxy) 3,3 of 1,1-, 5-trimethyl-cyclohexane 0.5 gram, therein ethylene base and organo-silicone rubber mass ratio are 0.06: 1.Stir desolvation after 30 minutes after adding superoxide, then be warming up to 155
oC reaction 20 minutes prepares the organosilicon thermoplastic elastomer, 90 ℃ of products therefrom softening temperatures, tensile strength 3.12MPa, elongation at break 210%.
Embodiment 5
Under 25 ℃ of conditions, 20 grams are contained the phenyl of the methyl of vinyl/ethyl silicon rubber and 20 grams/propyl group silicon rubber to be dissolved in the mixing of 250 ml toluene and tetrahydrofuran (THF), MQ resin 400 grams that contain vinyl that add again molecular weight 11500, TD silicone resin 30 grams of molecular weight 9000, add after mixing and contain hydrogen containing siloxane 4 grams and Platinic chloride 0.5 gram and 1, two (t-butyl peroxy) 3 of 1-, 3,5-trimethyl-cyclohexane 1.5 grams, therein ethylene base and organo-silicone rubber mass ratio are 0.12: 1.Stir desolvation after 30 minutes after adding superoxide, then be warming up to 150
oC reaction 10 minutes prepares the organosilicon thermoplastic elastomer, 90 ℃ of products therefrom softening temperatures, tensile strength 3.85MPa, elongation at break 150%.
Embodiment 6
the methyl silicone rubber that 200 grams is contained vinyl, 10 grams contain the methyl silicone rubber of propenyl, 20 gram phenyl siloxane rubbers and 500 gram molecular weights 11000 contain the MQ resin of vinyl, the TD resin of 25 gram molecular weights 4600 and hydrogen containing siloxane 12 grams and Platinic chloride 0.1 gram join in twin screw extruder, wherein containing thiazolinyl organic group and organo-silicone rubber mass ratio is 0.05: 1, extrude under 150 ℃ of conditions and prepare the organosilicon thermoplastic elastomer, the time that material stops in twin screw extruder is 3 minutes, 100 ℃ of products therefrom softening temperatures, draw high intensity 2.5 MPa, elongation at break 300%
Embodiment 7
220 grams are contained vinyl methyl machine silicon rubber, 10 grams contain the methyl silicone rubber of propenyl, 20 gram phenyl siloxane rubbers and 1000 gram molecular weights 9000 contain the MQ resin of vinyl, and hydrogen containing siloxane 5 grams and Platinic chloride 0.02 gram and 2, 5-dimethyl-2, 5 two (t-butyl peroxy) hexane, 1.5 grams join in twin screw extruder, wherein containing the organo-functional group of thiazolinyl and the mass ratio of organo-silicone rubber is 0.035: 1, the organosilicon thermoplastic elastomer is directly extruded under 150 ℃ of conditions and is prepared, 77 ℃ of products therefrom softening temperatures, draw high intensity 1.6 MPa, elongation at break 320%.
Embodiment 8
the methyl silicone rubber that 300 grams is contained the vinyl thiazolinyl, 40 gram phenyl siloxane rubbers and 1500 gram molecular weights 7000 contain the MQ resin of vinyl, the MT resin of 15 gram molecular weights 5000, the MTD resin of 15 gram molecular weights 8 000 and hydrogen containing siloxane 12 grams and Platinic chloride 0.01 gram and 2, 5-dimethyl-2, 5 two (t-butyl peroxy) hexane, 1.5 grams join in kneader, wherein containing the organo-functional group of thiazolinyl and the mass ratio of organo-silicone rubber is 0.085: 1, the organosilicon thermoplastic elastomer is mediated under 120 ℃ of conditions and was prepared in 2 hours, 90 ℃ of products therefrom softening temperatures, draw high intensity 2.8 MPa, elongation at break 260%.
Embodiment 9
the phenyl siloxane rubber that 150 grams is contained the vinyl thiazolinyl, contain 10 grams allylic methyl silicone rubber and 500 gram molecular weights 8800 contain the MQ resin of vinyl, the MT resin and 2 of 200 gram molecular weights 7600, 5-dimethyl-2, 5 two (t-butyl peroxy) hexane 6 grams and 2, 5-dimethyl-2, 5-two (t-butyl peroxy) acetylene 0.2 gram joins in kneader, wherein containing the organo-functional group of thiazolinyl and the mass ratio of organo-silicone rubber is 0.075: 1, the organosilicon thermoplastic elastomer is mediated under 150 ℃ of conditions and was prepared in 2 hours, 140 ℃ of products therefrom softening temperatures, draw high intensity 3.8 MPa, elongation at break 210%.
Claims (10)
1. an organosilicon thermoplastic elastomer, is characterized in that the starting raw material of this thermoplastic elastomer is composed of the following components, counts by weight:
100 parts of organo-silicone rubbers
Silicone resin 50-2000 part
Cross-linking system 0.08-30 part.
2. organosilicon thermoplastic elastomer according to claim 1 is characterized in that organo-silicone rubber is the organopolysiloxane of linearity or branching, its chemical structural formula:
(R
1 3SiO
1/2)
x(R
2 2SiO
2/2)
y(R
3SiO
3/2)
z
Wherein, x and y are 1～1000 positive integer, and z is 0 or 1～1000 positive integer;
R
1, R
2And R
3Be hydrogen, amino, phenyl, C
1-20Alkyl, C
1-20Alkyl phenyl, C
1-20Alkoxyl group or contain C
2-8Identical or different organic group in thiazolinyl.
3. organosilicon thermoplastic elastomer according to claim 1 is characterized in that the chemical structural formula of silicone resin is:
R
4 3SiO
1/2Unit and SiO
4/2The MQ resin of unit, or contain R
5SiO
3/2Unit and R
6 2SiO
2/2The TD resin of unit, or contain R
4 3SiO
1/2Unit and R
5SiO
3/2The MT resin of unit, or contain R
4 3SiO
1/2Unit, R
5SiO
3/2Unit and R
6 2SiO
2/2At least a in the MTD resin of unit;
R wherein
4, R
5And R
6Be hydrogen, amino, phenyl, C
1-20Alkyl, C
1-20Alkyl phenyl, C
1-20Alkoxyl group or contain C
2-8Identical or different organic group in thiazolinyl.
4. according to claim 2 or 3 described organosilicon thermoplastic elastomers, is characterized in that: in the mixture that organo-silicone rubber and silicone resin form, need comprise at least 2 organic groups that contain thiazolinyl; The described organic group that contains thiazolinyl is provided by organo-silicone rubber or is provided or by both jointly providing, the organic group and the organo-silicone rubber mass ratio that contain thiazolinyl are 0.0005 ~ 0.20: 1 by silicone resin.
5. organosilicon thermoplastic elastomer according to claim 1 is characterized in that described cross-linking system is organo-peroxide or/and at least a or two in organic hydrogen polysiloxanes.
6. organosilicon thermoplastic elastomer according to claim 5, it is characterized in that organo-peroxide is 1, two (t-butyl peroxy) 3 of 1-, 3,5-trimethyl-cyclohexane, 2,5-dimethyl-2,5 two (t-butyl peroxy) hexane and 2,5-dimethyl-2, at least a in 5-two (t-butyl peroxy) acetylene.
7. require 5 described organosilicon thermoplastic elastomers according to profit, it is characterized in that organic hydrogen polysiloxanes is the organopolysiloxane that contains at least two silicon-hydrogen bonds.
8. organosilicon thermoplastic elastomer according to claim 5, it is characterized in that also comprising in cross-linking system catalyzer, described catalyzer is that the complex compound, four (triphenylphosphine) of Platinic chloride or Platinic chloride and vinylsiloxane closes at least a in palladium and three (triphenylphosphine) rhodium chloride, wherein, the quality ratio of catalyzer and organo-silicone rubber is 0 – 0.03: 1.
9. one of according to claim 1 ~ 8 described organosilicon process for preparation of thermoplastic elastomer is characterized in that the method comprises the following steps:
(1) 30 parts of 100 parts of organo-silicone rubbers, silicone resin 50-2000 part, cross-linking system 0.08-are mixed in solvent or mixing machine;
(2) mixed 2～300 minutes 20-250 ℃ of temperature, obtain 150 ℃ of glass transition 70 – of organic thermoplastic elastic;
Wherein organic solvent is at least a in toluene, dimethylbenzene, tetrahydrofuran (THF), methylene dichloride.
10. organosilicon process for preparation of thermoplastic elastomer according to claim 9, is characterized in that mixing machine is any in opening rubber mixing machine or internal rubber mixer or closed kneader or screw extrusion press.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106188546A (en) * | 2016-07-20 | 2016-12-07 | 上海玉城高分子材料股份有限公司 | A kind of polystyrene anti-impact plasticized modifier and preparation method thereof |
| CN108865053A (en) * | 2018-08-01 | 2018-11-23 | 深圳日高胶带新材料有限公司 | A kind of high-low temperature resistant conduction organic pressure-sensitive gel and the preparation method and application thereof |
| US20210395527A1 (en) * | 2018-12-29 | 2021-12-23 | Shandong Branden Medical Device Co.,Ltd | Medical silicon rubber having high mechanical property and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993589A (en) * | 2009-08-13 | 2011-03-30 | 深圳市沃尔核材股份有限公司 | Silicon rubber shrinkable tube and preparation method thereof |
-
2013
- 2013-04-10 CN CN201310121908.3A patent/CN103160130B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993589A (en) * | 2009-08-13 | 2011-03-30 | 深圳市沃尔核材股份有限公司 | Silicon rubber shrinkable tube and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106188546A (en) * | 2016-07-20 | 2016-12-07 | 上海玉城高分子材料股份有限公司 | A kind of polystyrene anti-impact plasticized modifier and preparation method thereof |
| CN108865053A (en) * | 2018-08-01 | 2018-11-23 | 深圳日高胶带新材料有限公司 | A kind of high-low temperature resistant conduction organic pressure-sensitive gel and the preparation method and application thereof |
| CN108865053B (en) * | 2018-08-01 | 2021-01-29 | 深圳日高胶带新材料有限公司 | High-low temperature resistant conductive organic silicon pressure-sensitive adhesive and preparation method and application thereof |
| US20210395527A1 (en) * | 2018-12-29 | 2021-12-23 | Shandong Branden Medical Device Co.,Ltd | Medical silicon rubber having high mechanical property and preparation method thereof |
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