CN117070070A - Low-density high-mechanical-property silicone rubber foam material and preparation method thereof - Google Patents
Low-density high-mechanical-property silicone rubber foam material and preparation method thereof Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 49
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 45
- 239000006261 foam material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229920002545 silicone oil Polymers 0.000 claims abstract description 167
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 125
- 239000001257 hydrogen Substances 0.000 claims abstract description 125
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 117
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 72
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 38
- 229920001971 elastomer Polymers 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 25
- 238000004073 vulcanization Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 239000006260 foam Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 229910052697 platinum Inorganic materials 0.000 claims description 19
- 229910021485 fumed silica Inorganic materials 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 16
- 239000000945 filler Substances 0.000 claims description 16
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 15
- 239000003112 inhibitor Substances 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 7
- 239000000347 magnesium hydroxide Substances 0.000 claims description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 4
- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- IEPRKVQEAMIZSS-AATRIKPKSA-N diethyl fumarate Chemical compound CCOC(=O)\C=C\C(=O)OCC IEPRKVQEAMIZSS-AATRIKPKSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003446 ligand Substances 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 3
- -1 vinyl siloxane Chemical class 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 abstract description 12
- 230000006835 compression Effects 0.000 abstract description 6
- 238000007906 compression Methods 0.000 abstract description 6
- 150000002431 hydrogen Chemical class 0.000 abstract description 3
- 229920002323 Silicone foam Polymers 0.000 abstract 2
- 239000013514 silicone foam Substances 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 18
- 229910002027 silica gel Inorganic materials 0.000 description 8
- 239000000741 silica gel Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000003490 calendering Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/02—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by the reacting monomers or modifying agents during the preparation or modification of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of organic silicon foam materials, and particularly relates to a low-density high-mechanical-property silicon rubber foam material and a preparation method thereof. The thickness of the low-density high-mechanical-property silicone rubber foam material formed in the invention is 0.5-6 mm, and the density is 450-950 kg/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The tensile strength of the silicone rubber foam material is 0.8-1.6 MPa, the 25% compressive stress is 0.1-0.4 MPa, and the elongation at break is more than or equal to 80%. The invention is realized by combining different structuresThe silicone oil containing hydrogen is compounded, and the side chain hydrogen silicone oil with low hydrogen content is particularly added to increase active crosslinking points and promote local crosslinking degree, so that the silicone foam with low density and high tensile strength is formed, and meanwhile, the polyvinyl silicone oil is added to strengthen the compression stress of the silicone foam, so that the silicone rubber foam material with low density and high mechanical property is obtained.
Description
Technical Field
The invention belongs to the technical field of organic silicon foam materials, and particularly relates to a low-density high-mechanical-property silicon rubber foam material and a preparation method thereof.
Background
At present, the silicone rubber foam is used as a heat insulation material, a sealing material, a buffer material and the like in various industries. With the rapid development of new energy automobiles, the battery soft package material has higher requirements on the silicone rubber foam material. The conventional low-density silicon rubber has low tensile strength and low compression stress, and the silicon rubber with high tensile strength and high compression stress is high in density, so that the buffering and damping functions are lost, and the requirements of light weight and high mechanical properties of the battery for the new energy automobile cannot be met. There is a need to obtain a silicone rubber foam material that combines low density with high mechanical properties, including tensile strength, compressive stress, and elongation at break.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a silicone rubber foam material with low density, high tensile strength and high compressive stress and a preparation method thereof.
In order to achieve the above object, the present invention provides a silicone rubber foam material with low density, high tensile strength and high compressive stress, comprising a material A and a material B;
the material A comprises, by mass, 80-160 parts of vinyl-terminated silicone oil, 25-75 parts of rubber compound, 30-60 parts of hydroxyl-terminated silicone oil, 2-10 parts of polyvinyl silicone oil, 3-6 parts of platinum catalyst and 60-150 parts of filler;
the material B comprises, by mass, 70-140 parts of vinyl-terminated silicone oil, 50-100 parts of rubber compound, 10-60 parts of mixed hydrogen-containing silicone oil, 2-10 parts of polyvinyl silicone oil, 0.1-1 part of inhibitor and 60-150 parts of filler.
Further, the thickness of the silicone rubber foam material is 0.5-6 mm, and the density is 450-950 kg/m 3 The tensile strength is 0.8-1.6 MPa, the 25% compressive stress is 0.1-0.4 MPa, and the elongation at break is more than or equal to 80%.
Further, the viscosity of the vinyl-terminated silicone oil is 5000-200000 mPas, preferably 10000-100000 mPas, wherein the mass percentage of vinyl is 0.02-1.0%;
the rubber compound comprises the vinyl-terminated silicone oil and fumed silica, wherein the mass ratio of the fumed silica in the rubber compound is 20% -45%; the specific surface area of the fumed silica in the rubber compound is200～480m 2 /g。
Further, the hydroxyl group content of the hydroxyl group-terminated silicone oil is 3.0 to 8.0% by mass, and the viscosity of the hydroxyl group-terminated silicone oil is 5 to 100 mPas, more preferably 25 to 50 mPas.
Further, the viscosity of the polyvinyl silicone oil is 1000 to 12000 mPas, more preferably 1000 to 3000 mPas, and the mass percentage of the vinyl group contained therein is 1.0 to 10.0%.
Further, the platinum catalyst is at least one of tetrahydrofuran coordinated platinum catalyst, isopropanol coordinated chloroplatinic acid catalyst, chloroplatinic acid-diethyl phthalate complex solution and platinum complex containing vinyl siloxane ligand; the mass percentage of the platinum catalyst in the silicone rubber foam material is (1-30) multiplied by 10 -4 wt％。
Further, the mixed hydrogen-containing silicone oil comprises hydrogen-containing silicone oil H1, hydrogen-containing silicone oil H2 and hydrogen-containing silicone oil H3; the mass ratio of the hydrogen-containing silicone oil H1 to the hydrogen-containing silicone oil H2 to the hydrogen-containing silicone oil H3 is 1: (0.1-0.3): (0.1-0.3), the hydrogen content of the hydrogen-containing silicone oil H1 is 0.25-1.0 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H2 is 1.2 to 1.6 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H3 is 0.18 to 0.25 percent by mass;
the hydrogen-containing silicone oil H1 and the hydrogen-containing silicone oil H2 are both methyl-terminated side chain hydrogen-containing silicone oil, and the hydrogen-containing silicone oil H3 is hydrogen-terminated low hydrogen-containing silicone oil; the viscosity of the hydrogen-containing silicone oil H1 is 25 to 1000 mPas, more preferably 50 to 200 mPas, and the viscosity of the hydrogen-containing silicone oil H2 is 5 to 200 mPas, more preferably 10 to 120 mPas; the viscosity of the hydrogen-containing silicone oil H3 is 25 to 1000 mPas, more preferably 50 to 300 mPas.
Further, the inhibitor is at least one of 2-methyl-3-alkyne-2-ol, 3-methyl-1-alkyne-3-ol, ethynyl cyclohexanol, diallyl maleate and diethyl fumarate; the dosage of the inhibitor is 0.01 to 0.1 weight percent of the silicone rubber foam material;
the filler comprises at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, silicon micropowder, mica powder and talcum powder; the median particle diameter of the filler is 1-50 mu m.
According to another aspect of the present invention, there is provided a method for preparing the silicone rubber foam material, comprising the steps of:
s1: mixing and stirring all the components of the material A uniformly to obtain a uniformly dispersed material A;
s2: mixing and uniformly stirring all the components of the material B to obtain a uniformly dispersed material B;
s3: mixing the uniformly dispersed material A and the uniformly dispersed material B, and uniformly stirring to obtain a mixed material;
s4: and (3) coating the mixed material in the step (S3) on a film, performing first-stage low-temperature vulcanization, and then performing second-stage high-temperature vulcanization to obtain the low-density high-tensile-strength high-compression-stress silicone rubber foam material.
Further, the vulcanization temperature of the first section of vulcanization in the step S4 is 70-90 ℃ and the vulcanization time is 1-5 min; the second stage of vulcanization has the vulcanization temperature of 150-200 ℃ and the vulcanization time of 10-40 min.
In general, the above technical solutions conceived by the present invention have the following compared with the prior art
The beneficial effects are that:
(1) According to the silicone rubber foam material with low density, high tensile strength and high compression stress, the hydrogen-containing silicone oil with different structures and hydrogen content is compounded, and the side chain hydrogen-containing silicone oil with low hydrogen content is particularly added, so that active crosslinking points are increased, and the local crosslinking degree is improved. Under the action of a platinum catalyst, the low-hydrogen silicone oil and the vinyl-terminated silicone oil are subjected to crosslinking reaction, and simultaneously react with the hydroxyl-terminated silicone oil to release hydrogen, so that compact closed micropores are formed, the silica gel foam with low density and high tensile strength is formed, and the compressive stress of the silica gel foam can be enhanced by adding proper amount of the polyvinyl silicone oil.
(2) Unlike common silicone rubber, the silicone rubber foam material of the invention is added with low-viscosity hydrogen-containing silicone oil (comprising hydroxyl-terminated silicone oil and mixed hydrogen-containing silicone oil) in a certain proportion, so that the viscosity of the rubber material is low, the filler is easy to fully disperse, and bubbles mixed in the stirring and dispersing process are easy to be pumped and discharged from the rubber material. Because the viscosity is low and the fluidity is good, the two material components can be quickly mixed in the quick mixing and coating calendaring process, the mixing temperature is easy to control, and the influence on the coating effect caused by the cross-linking foaming reaction in advance due to the sudden rise of the temperature of the mixed material caused by a large amount of heat generated in the quick mixing process is avoided. The surface grain of the silicone rubber prepared by coating after rapid mixing is easy to control, and the consistency of the product is good.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a low-density high-tensile-strength high-compression-stress silicone rubber foam material, which comprises a material A and a material B; the material A comprises, by mass, 80-160 parts of vinyl-terminated silicone oil, 25-75 parts of rubber compound, 30-60 parts of hydroxyl-terminated silicone oil, 2-10 parts of polyvinyl silicone oil, 3-6 parts of platinum catalyst and 60-150 parts of filler; the material B comprises, by mass, 70-140 parts of vinyl-terminated silicone oil, 50-100 parts of rubber compound, 10-60 parts of mixed hydrogen-containing silicone oil, 2-10 parts of polyvinyl silicone oil, 0.1-1 part of inhibitor and 60-150 parts of filler.
According to the invention, the thickness of the silicone rubber foam material can be provided with the thickness of 0.5-6 mm, generally 1mm, 2mm and 5mm; the density is 450-950 kg/m 3 The tensile strength is 0.8-1.6 MPa, the 25% compressive stress is 0.1-0.4 MPa, and the elongation at break is more than or equal to 80%.
In some embodiments, the vinyl-terminated silicone oil has a viscosity of 5000-200000 mPas, more preferably 10000-100000 mPas, and a vinyl content of 0.02-1.0% by mass; the rubber compound comprises the vinyl-terminated silicone oil and fumed silica, wherein the mass ratio of the fumed silica in the rubber compound is 20% -45%; the specific surface area of the fumed silica in the rubber compound is 200-480 m 2 And/g. The hydroxyl-terminated silicone oil contains hydroxyl groupsThe mass percentage is 3.0-8.0%, and the viscosity of the hydroxyl-terminated silicone oil is 5-100 mPas, more preferably 25-50 mPas. The viscosity of the polyvinyl silicone oil is 1000-12000 mPas, more preferably 1000-3000 mPas, and the mass percentage of the vinyl contained in the polyvinyl silicone oil is 1.0-10.0%.
In some embodiments, the platinum catalyst is at least one of a tetrahydrofuran coordinated platinum catalyst, an isopropanol coordinated chloroplatinic acid catalyst, a chloroplatinic acid-diethyl phthalate complex solution, and a platinum complex containing a vinyl siloxane ligand; the mass percentage of the platinum catalyst in the silicone rubber foam material is (1-30) multiplied by 10 -4 wt％。
In some embodiments, the mixed hydrogen-containing silicone oil includes hydrogen-containing silicone oil H1, hydrogen-containing silicone oil H2, and hydrogen-containing silicone oil H3; the mass ratio of the hydrogen-containing silicone oil H1 to the hydrogen-containing silicone oil H2 to the hydrogen-containing silicone oil H3 is 1: (0.1-0.3): (0.1-0.3), the hydrogen content of the hydrogen-containing silicone oil H1 is 0.25-1.0 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H2 is 1.2 to 1.6 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H3 is 0.18 to 0.25 percent by mass; the hydrogen-containing silicone oil H1 and the hydrogen-containing silicone oil H2 are both methyl-terminated side chain hydrogen-containing silicone oil, and the hydrogen-containing silicone oil H3 is hydrogen-terminated low hydrogen-containing silicone oil; the viscosity of the hydrogen-containing silicone oil H1 is 25 to 1000 mPas, more preferably 50 to 200 mPas, and the viscosity of the hydrogen-containing silicone oil H2 is 5 to 200 mPas, more preferably 10 to 120 mPas; the viscosity of the hydrogen-containing silicone oil H3 is 25 to 1000 mPas, more preferably 50 to 300 mPas. Specifically, the hydrogen-containing silicone oil can be purchased from Zhejiang Xin An chemical group Co., shandong Dong chemical Co., hesheng silicon Co., daokanning, xinyue, michaelia and other companies selling chemical products.
In some embodiments, the inhibitor is at least one of 2-methyl-3-yn-2-ol, 3-methyl-1-yn-3-ol, ethynyl cyclohexanol, diallyl maleate, diethyl fumarate; the dosage of the inhibitor is 0.01 to 0.1 weight percent of the silicone rubber foam material; the filler comprises at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, silicon micropowder, mica powder and talcum powder; the median particle diameter of the filler is 1-50 mu m.
The invention also provides a preparation method of the silicone rubber foam material, which comprises the following steps:
s1: mixing and stirring all the components of the material A uniformly to obtain a uniformly dispersed material A;
s2: mixing and uniformly stirring all the components of the material B to obtain a uniformly dispersed material B;
s3: mixing the uniformly dispersed material A and the uniformly dispersed material B, and uniformly stirring to obtain a mixed material;
s4: and (3) coating the mixed material in the step (S3) on a film, performing first-stage low-temperature vulcanization, and then performing second-stage high-temperature vulcanization to obtain the low-density high-tensile-strength high-compression-stress silicone rubber foam material.
In some embodiments, the rotational speed of stirring and dispersing the material A in the step S1 is 800-2000 r/min, specifically, may be 1000r/min; the stirring and dispersing time is 5-45 min, specifically 30min. In the step S2, the rotation speed of stirring and dispersing the material B is 800-2000 r/min, and specifically, can be 1000r/min; the stirring and dispersing time is 5 to 45 minutes, and specifically may be 25 minutes. In the step S3, the materials A and B are uniformly mixed, and the stirring rotating speed is 50-300 r/min, specifically, 300r/min; the stirring time is 3 to 10 minutes, specifically, may be 5 minutes. And step S3, mixing the material A and the material B to ensure that the mixing temperature is controlled below 50 ℃.
In some embodiments, the first stage of vulcanization in step S4 has a vulcanization temperature of 70-90 ℃ and a vulcanization time of 1-5 min; the second stage of vulcanization has the vulcanization temperature of 150-200 ℃ and the vulcanization time of 10-40 min.
The methyl-terminated side chain hydrogen-containing silicone oil and the hydrogen-terminated low hydrogen-containing silicone oil are particularly added into the silicone rubber foam material, and active crosslinking points are increased and local crosslinking degree is improved through compounding of different hydrogen-containing silicone oils. Under the action of a platinum catalyst, the low-hydrogen silicone oil and the vinyl-terminated silicone oil are subjected to crosslinking reaction, and simultaneously react with the hydroxyl-terminated silicone oil to release hydrogen, so that compact closed micropores are formed, the silica gel foam with low density and high tensile strength is formed, and the compressive stress of the silica gel foam can be enhanced by adding proper amount of the polyvinyl silicone oil.
Specifically, the hydrogen-containing silicone oil H1 has a low hydrogen content and is a silicone oil having a hydrogen-containing side chain. Because the silicon oil with low hydrogen content contains less Si-H bonds, under the condition of a certain total mole number of Si-H bonds, the more the added silicon oil with low hydrogen content is, the more the side chain hydrogen-containing silicon oil in the material is, the more active crosslinking points are, the side chain hydrogen-containing silicon oil reacts with vinyl silicon oil to form a branched chain staggered network structure, so that the local crosslinking degree of the silicon gel is improved; the hydrogen-containing silicone oil H2 is hydrogen-containing silicone oil with more hydrogen in a side chain, has higher activity, is easier to react with hydroxyl silicone oil to form uniform and compact cells, and increases the foaming ratio of the silica gel; the hydrogen-containing silicone oil H3 is low hydrogen-containing silicone oil with hydrogen at the end, and a small amount of the hydrogen-containing silicone oil at the end is added to react with vinyl silicone oil to increase the chain length, so that the chain extension effect is achieved, and the silica gel foam is ensured to have certain toughness. The preferable proportioning mode of the three hydrogen-containing silicone oils can ensure that the silicone rubber foam has low density and high tensile strength and high compression stress. Meanwhile, the polyvinyl silicone oil can strengthen the compression stress of the silica gel foam, and a certain amount of polyvinyl silicone oil with relatively concentrated partial vinyl groups is added, namely, when the polyvinyl silicone oil with relatively concentrated side chain containing parts and the hydrogen-containing silicone oil are vulcanized, a plastic micro-area with larger strength can be generated, and the internal concentrated crosslinking is increased, so that the tensile strength of the silica gel is improved.
On the other hand, since the low-hydrogen silicone oil contains a small amount of Si-H bonds, when the total number of moles of Si-H bonds is constant, the viscosity of the low-hydrogen silicone oil is 50 to 300 mPas, the viscosity of the vinyl-terminated silicone oil is 10000 to 100000 mPas, and the amount of the low-hydrogen silicone oil to be added increases, which corresponds to an increase in the amount of the low-viscosity silicone oil to be added, and the total material viscosity decreases. The low viscosity of the total material is beneficial to the processing technology, and the surface mark is easy to control.
The following are examples:
the average viscosity of the vinyl-terminated silicone oil in the following example 1 and comparative examples 1 to 5 was 20000mpa·s, the mass percentage of vinyl groups was 0.3%; the rubber compound contains the vinyl-terminated silicone oil and the fumed silica, wherein the fumed silica is arranged in the rubber compoundThe mass ratio of (2) is 30%; the specific surface area of the fumed silica in the rubber compound is 300m 2 /g; the mass percentage of hydroxyl in the hydroxyl-terminated silicone oil is 3 percent, and the average viscosity is 40 mPa.s; the average viscosity of the polyvinyl silicone oil is 2000 mPas, and the mass percentage of vinyl is 5%; the platinum catalyst is a chloroplatinic acid catalyst coordinated with isopropanol, the hydrogen-containing silicone oil H1 is methyl end-capped side chain low hydrogen-containing silicone oil, the weight percentage of H is 0.5%, the average viscosity is 180 mPas, the hydrogen-containing silicone oil H2 is methyl end-capped side chain hydrogen-containing silicone oil, the weight percentage of H is 1.5%, the average viscosity is 20 mPas, the hydrogen-containing silicone oil H3 is hydrogen end-capped low hydrogen-containing silicone oil, the weight percentage of H is 0.20%, the average viscosity is 260 mPas, and the inhibitor is diallyl maleate.
The vinyl-terminated silicone oils used in examples 2 and 3 had an average viscosity of 10000 mPas and a vinyl content of 0.5% by mass; the rubber compound comprises the vinyl-terminated silicone oil and fumed silica, wherein the mass ratio of the fumed silica in the rubber compound is 40%; the specific surface area of the fumed silica in the rubber compound is 250m 2 /g; the mass percentage of hydroxyl in the hydroxyl-terminated silicone oil is 6%; the average viscosity of the polyvinyl silicone oil is 1000 mPas, and the mass percentage of vinyl is 8%; the inhibitor was 3-methyl-1-yn-3-ol, otherwise as in example 1.
The vinyl-terminated silicone oils used in examples 4 and 5 had an average viscosity of 40000 mPas and a vinyl content of 0.1% by mass; the rubber compound comprises the vinyl-terminated silicone oil and fumed silica, wherein the mass ratio of the fumed silica in the rubber compound is 20%; the specific surface area of the fumed silica in the rubber compound is 450m 2 /g; the mass percentage of hydroxyl in the hydroxyl-terminated silicone oil is 4%; the average viscosity of the polyvinyl silicone oil is 3000 mPas, and the mass percentage of vinyl is 2%; the inhibitor was 2-methyl-3-yn-2-ol, otherwise as in example 1.
Example 1
S1) preparation of a material A: the material A is prepared by the following raw materials in parts by weight, wherein 132 parts of vinyl-terminated silicone oil, 50 parts of rubber compound, 40 parts of hydroxyl-terminated silicone oil with the hydroxyl mass percentage content of 3.0%, 4 parts of polyvinyl silicone oil, 4 parts of platinum catalyst and 70 parts of filler (the mass ratio of magnesium hydroxide to magnesium hydroxide is 1:1, and the median particle size of the filler is 20 mu m), and the materials are mixed in a disperser at the dispersing speed of 1000r/min for 45 min;
s2) preparation of a material B: the material B is prepared by the following raw material formulas in parts by mass, 107 parts of vinyl-terminated silicone oil, 90 parts of rubber compound, 29.6 parts of mixed hydrogen-containing silicone oil (wherein the hydrogen-containing silicone oil H1, the hydrogen-containing silicone oil H2, the hydrogen-containing silicone oil H3 and the 3.1 parts by mass are respectively 23.1 parts, 3.5 parts and 3.0 parts), 4 parts of polyvinyl silicone oil, 0.2 part of inhibitor and 70 parts of filler (the mass ratio of magnesium hydroxide to magnesium hydroxide is 1:1, and the median particle size of the filler is 20 mu m), and the materials are mixed in a disperser at a dispersing speed of 1000r/min and stirring time of 35 min;
s3) stirring the material A and the material B for 10min at the stirring speed of a screw rod of 300r/min to obtain a mixed material;
s4) coating the mixture on a PET film, wherein the coating thickness is 2mm, baking and vulcanizing for 3min at 80 ℃, and transferring to 150 ℃ for baking and vulcanizing for 25min to obtain the silicone rubber foam.
Comparative example 1
S1) preparation of a material A: the composite material is prepared from the following raw materials in parts by mass; mixing in a disperser at a dispersing speed of 1000r/min for 45min to obtain a material A;
s2) preparation of a material B: the adhesive is prepared from the following raw materials in parts by mass; mixing in a disperser at a dispersing speed of 1000r/min for 35min to obtain a material B;
s3) stirring the materials A and B for 10min at the stirring speed of a screw rod of 300r/min to obtain a mixed material;
s4) coating the mixture on a PET film, wherein the coating thickness is 2mm, baking and vulcanizing for 3min at 80 ℃, and transferring to 150 ℃ for baking and vulcanizing for 25min to obtain the silicone rubber foam.
Comparative example 2
S1) preparation of a material A: the modified polyurethane is prepared from the following raw materials in parts by mass; mixing in a disperser at a dispersing speed of 1000r/min for 45min to obtain a material A;
s2) preparation of a material B: the adhesive is prepared from the following raw materials in parts by mass; mixing in a disperser at a dispersing speed of 1000r/min for 35min to obtain a material B;
s3) stirring the materials A and B for 10min at a stirring speed of 300r/min to obtain a mixed material;
s4) coating the mixture on a PET film, wherein the coating thickness is 2mm, baking and vulcanizing for 5min at 90 ℃, and transferring to 200 ℃ for baking and vulcanizing for 40min to obtain the silicone rubber.
Table 1 composition of materials for each of examples and comparative examples
Table 2 analysis of results for each of the comparative and example silicone rubber foams
As can be seen from tables 1 and 2, comparative example 1, comparative example 3 and comparative example 4 changed the amount distribution of the three hydrogen-containing silicone oils with respect to the examples, wherein the mass ratio of the hydrogen-containing silicone oil H1, the hydrogen-containing silicone oil H2 and the hydrogen-containing silicone oil H3 of comparative example 1 was 3:15:4; comparative example 3 the mass ratio of hydrogen containing silicone oil H1, hydrogen containing silicone oil H2 and hydrogen containing silicone oil H3 is 42:3.5:4.5, which is much higher than the addition ratio of hydrogen containing silicone oil H2 in the examples; the mass ratio of the hydrogen-containing silicone oil H1, the hydrogen-containing silicone oil H2 and the hydrogen-containing silicone oil H3 in comparative example 4 is 21:5:14, which is far higher than the addition ratio of the hydrogen-containing silicone oil H3 in examples. As can be seen from tables 1 and 2, comparative example 2 does not add hydroxyl-terminated silicone oil; comparative example 5 has an excessive vinyl group added, which is far higher than the amount of the polyvinyl silicone oil added in the examples. From the results of the mechanical property test, the thickness of the silicone rubber foam materials of examples 1 to 5 is 2.5 to 2.8mm, and the density is 462 to 905kg/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The tensile strength is 0.85-1.54 MPa, the 25% compressive stress is 0.12-0.35 MPa, and the elongation at break is more than 84%; comparative example 1, although having a lower density, has lower tensile strength and lower compressive stress; comparative example 2 has 25% compressive stress as high as 2.62MPa and density as high as 1530kg/m 3 The foam cushion has no buffering and damping effects; comparative example 3 has lower tensile strength, compressive stress and elongation at break than the examples; the tensile strength and the compressive stress of the comparative example 4 are lower than those of the examples although the elongation at break is as high as 116%; comparative example 5 has a higher tensile strength and higher compressive stress, but has a lower elongation at break than the examples.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A low-density high-tensile-strength high-compressive-stress silicone rubber foam material is characterized by comprising a material A and a material B;
the material A comprises, by mass, 80-160 parts of vinyl-terminated silicone oil, 25-75 parts of rubber compound, 30-60 parts of hydroxyl-terminated silicone oil, 2-10 parts of polyvinyl silicone oil, 3-6 parts of platinum catalyst and 60-150 parts of filler;
the material B comprises, by mass, 70-140 parts of vinyl-terminated silicone oil, 50-100 parts of rubber compound, 10-60 parts of mixed hydrogen-containing silicone oil, 2-10 parts of polyvinyl silicone oil, 0.1-1 part of inhibitor and 60-150 parts of filler.
2. The silicone rubber foam according to claim 1, wherein the thickness of the silicone rubber foam is 0.5-6 mm and the density is 450-950 kg/m 3 The tensile strength is 0.8-1.6 MPa, the 25% compressive stress is 0.1-0.4 MPa, and the elongation at break is more than or equal to 80%.
3. The silicone rubber foam material according to claim 1, wherein the vinyl-terminated silicone oil has a viscosity of 5000 to 200000 mPa-s, wherein the mass percentage of vinyl groups is 0.02 to 1.0%;
the rubber compound comprises the vinyl-terminated silicone oil and fumed silica, wherein the mass ratio of the fumed silica in the rubber compound is 20% -45%; the specific surface area of the fumed silica in the rubber compound is 200-450 m 2 /g。
4. The silicone rubber foam according to claim 1, wherein the hydroxyl-terminated silicone oil contains 3.0 to 8.0 mass% of hydroxyl groups and has a viscosity of 5 to 100 mPa-s.
5. The silicone rubber foam according to claim 1, wherein the polyvinyl silicone oil has a viscosity of 1000 to 12000 mPa-s and contains 1.0 to 10.0% by mass of vinyl groups.
6. The silicone rubber foam of claim 1, wherein the platinum catalyst is at least one of a tetrahydrofuran coordinated platinum catalyst, an isopropanol coordinated chloroplatinic acid catalyst, a chloroplatinic acid-diethyl phthalate complex solution, and a platinum complex containing vinyl siloxane ligands; the mass percentage of the platinum catalyst in the silicone rubber foam material is (1-30) multiplied by 10 -4 wt％。
7. The silicone rubber foam according to claim 1, wherein the mixed hydrogen-containing silicone oil comprises hydrogen-containing silicone oil H1, hydrogen-containing silicone oil H2, and hydrogen-containing silicone oil H3; the mass ratio of the hydrogen-containing silicone oil H1 to the hydrogen-containing silicone oil H2 to the hydrogen-containing silicone oil H3 is 1: (0.1-0.3): (0.1-0.3), the hydrogen content of the hydrogen-containing silicone oil H1 is 0.25-1.0 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H2 is 1.2 to 1.6 percent by mass; the hydrogen content of the hydrogen-containing silicone oil H3 is 0.18 to 0.25 percent by mass;
the hydrogen-containing silicone oil H1 and the hydrogen-containing silicone oil H2 are methyl-terminated side-chain low hydrogen-containing silicone oil, and the hydrogen-containing silicone oil H3 is hydrogen-terminated low hydrogen-containing silicone oil; the viscosity of the hydrogen-containing silicone oil H1 is 25-1000 mPa.s; the viscosity of the hydrogen-containing silicone oil H2 is 5-200 mPas; the viscosity of the hydrogen-containing silicone oil H3 is 25-1000 mPas.
8. The silicone rubber foam of claim 1, wherein the inhibitor is at least one of 2-methyl-3-yn-2-ol, 3-methyl-1-yn-3-ol, ethynyl cyclohexanol, diallyl maleate, diethyl fumarate; the dosage of the inhibitor is 0.01 to 0.1 weight percent of the silicone rubber foam material;
the filler comprises at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, silicon micropowder, mica powder and talcum powder.
9. A method of preparing a silicone rubber foam according to any one of claims 1 to 8, comprising the steps of:
s1: mixing and stirring all the components of the material A uniformly to obtain a uniformly dispersed material A;
s2: mixing and uniformly stirring all the components of the material B to obtain a uniformly dispersed material B;
s3: mixing the uniformly dispersed material A and the uniformly dispersed material B, and uniformly stirring to obtain a mixed material;
s4: and (3) coating the mixed material in the step (S3) on a film, performing first-stage low-temperature vulcanization, and then performing second-stage high-temperature vulcanization to obtain the low-density high-tensile-strength high-compression-stress silicone rubber foam material.
10. The method according to claim 9, wherein the first stage of vulcanization in step S4 has a vulcanization temperature of 70 to 90 ℃ and a vulcanization time of 1 to 5 minutes; the second stage of vulcanization has the vulcanization temperature of 150-200 ℃ and the vulcanization time of 10-40 min.
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