CN115216156B - Foamed silicone rubber sealing sheet and preparation method thereof - Google Patents
Foamed silicone rubber sealing sheet and preparation method thereof Download PDFInfo
- Publication number
- CN115216156B CN115216156B CN202211116016.XA CN202211116016A CN115216156B CN 115216156 B CN115216156 B CN 115216156B CN 202211116016 A CN202211116016 A CN 202211116016A CN 115216156 B CN115216156 B CN 115216156B
- Authority
- CN
- China
- Prior art keywords
- silicone rubber
- sealing sheet
- rubber sealing
- poss
- foamed silicone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
- B29B7/005—Methods for mixing in batches
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- 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
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of preparation of foamed silicone rubber sealing sheets, and discloses a foamed silicone rubber sealing sheet and a preparation method thereof, wherein the foamed silicone rubber sealing sheet is formed by punching a prepared foamed silicone rubber material through a cutting die, and the interior of the foamed silicone rubber sealing sheet comprises a circular cell structure with the average pore diameter distributed between 20 and 60 mu m, and the cells are independently closed-cell distributed; the formula of the foaming silicone rubber material is as follows: 100phr of vinyl silicone oil with the viscosity of 8000 mPas, 6 to 20phr of foaming auxiliary agent, 0.5 to 1.5phr of platinum catalyst with the content of 1000PPM, 0.1 to 0.4phr of inhibitor and 25 to 60phr of hydrogen-containing silicone oil with the hydrogen content of 0.12 percent; the foaming auxiliary agent is hydroxyl POSS terminated silica polymer, and the hydroxyl content of the foaming auxiliary agent is 3-7.7%; the foamed silicone rubber sealing sheet disclosed by the invention has excellent mechanical properties and also has good sealing performance.
Description
Technical Field
The invention relates to the technical field of preparation of foamed silicone rubber sealing sheets, in particular to a foamed silicone rubber sealing sheet and a preparation method thereof.
Background
The battery pack is an important component of a mechanical power device, and the safe and stable operation of the battery pack is a precondition for the safe and normal operation of a mechanical system. In order to prevent external water and corrosive substances from entering the battery, a sealing member is usually installed on the outer side of the battery pack to seal the battery, and the sealing member and the housing form a static sealing system.
The foaming silicone rubber is a porous polymer material prepared by taking silicone rubber as a matrix through a foaming process, combines the advantages of the silicone rubber and the foaming material, and has the characteristics of light weight, high and low temperature resistance, good insulativity and the like. The material has good following performance and super-elastic body characteristics, and is widely applied to static sealing of a battery shell as a sealing element.
Preparation method of foaming silicon rubber materialThe method comprises two methods of chemical foaming and physical foaming; wherein, by utilizing hydrosilylation and condensation reaction, under the action of a platinum catalyst, the catalyst contains Si-CH = CH 2 The bonded vinyl silicone oil and the hydrogen-containing silicone oil containing Si-H bonds are subjected to a cross-linking reaction, and the hydroxyl silicone oil containing Si-OH bonds and the hydrogen-containing silicone oil containing Si-H bonds generate foaming gas hydrogen to perform a foaming reaction to form the foaming silicone rubber material.
However, the foamed silicone rubber material prepared only by hydrosilylation and hydrosilylation condensation dehydrogenation reactions between silicone oils has the problems of high density, uncontrollable pressure-change performance and the like, and in order to solve the problems and prepare a light foamed silicone rubber material with uniform and controllable foam pores, there are reports in the literature that compounds containing hydroxyl groups, such as polyethylene glycol, polyhydric alcohol and the like, can be added into the foamed silicone rubber material, and the compounds containing hydroxyl groups can react with the silicone oil containing hydrogen, but the compounds containing hydroxyl groups cannot solve the problem of insufficient mechanical properties of the foamed silicone rubber material.
The research finds that: POSS has the technical effect of enhancing the mechanical property of the silicone rubber.
The following references are cited for the present invention: a doctor's academic paper on Nie Wang flame published in 2010 at Anhui university, POSS-based preparation and performance research of low-dielectric-constant nano porous silica film, discloses a structure and a preparation method of hydrogen-containing POSS (T8H 8).
The invention introduces POSS to improve the mechanical property of the foaming silicon rubber material.
Disclosure of Invention
Technical problem to be solved
The invention provides a foamed silicone rubber sealing sheet and a preparation method thereof.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a foamed silicone rubber sealing sheet is formed by punching a prepared foamed silicone rubber material through a cutting die, and the interior of the foamed silicone rubber sealing sheet comprises a circular cell structure with the average pore diameter distributed between 20 and 60 mu m, wherein the cells are independently closed-cell distributed;
wherein, the formula of the foaming silicon rubber material is as follows: 100phr of vinyl silicone oil with the viscosity of 8000 mPas, 6 to 20phr of foaming auxiliary agent, 0.5 to 1.5phr of platinum catalyst with the content of 1000PPM, 0.1 to 0.4phr of inhibitor and 25 to 60phr of hydrogen-containing silicone oil with the hydrogen content of 0.12 percent;
the foaming auxiliary agent is hydroxyl POSS terminated silica polymer, and the hydroxyl content of the foaming auxiliary agent is 3-7.7%.
Preferably, the foamed silicone rubber sealing sheet has a compressive stress of 90-120kPa for 25% compression, a compression set CS (50% compression, 22h,70 ℃) of 3.9-4.2%, and a water absorption of 1.4-1.5%.
Preferably, the preparation steps of the foamed silicone rubber sealing sheet are as follows:
step I, preparing a component I containing a catalyst, wherein the component I comprises the following raw materials: vinyl silicone oil, a foaming auxiliary agent, a platinum catalyst and an inhibitor, wherein the raw materials are uniformly dispersed by a homogenizer and then stored for later use;
step II, preparing a component II containing a cross-linking agent, wherein the component II comprises the following raw materials in formula: vinyl silicone oil and cross-linking agent-hydrogen-containing silicone oil, wherein the raw materials are uniformly dispersed by a homogenizer and then stored for later use;
step III, preparing the component I and the component II according to the mass ratio of 1;
and Step IV, placing the vulcanized foaming silicone rubber material into an oven at the temperature of 80-100 ℃ for constant temperature treatment for 12-15h, and punching the material into a foaming silicone rubber sealing sheet with the width of (600-605) mm and the thickness of (5 +/-0.3) mm by using a cutting die.
Preferably, the foaming auxiliary agent is a double-end hydroxyl POSS terminated silica polymer or a single-end hydroxyl POSS terminated silica polymer.
Preferably, the synthesis method of the double-end hydroxyl POSS terminated silica polymer comprises the following steps:
step1-1, taking hydrogen-containing POSS (T8H 8), p-divinylbenzene and tetramethyldisiloxane as reaction monomers, and synthesizing a double-ended hydrosilation POSS end-capped silica functional monomer through a hydrosilylation reaction;
step1-2, synthesizing a double-end hydroxyl POSS end-capped silica functional monomer by taking a double-end hydrosilation POSS end-capped silica functional monomer and 4-hydroxystyrene as reaction monomers through a hydrosilylation reaction;
and Step1-3, carrying out chain extension reaction on a double-end hydroxyl POSS end-capped silicon-oxygen functional monomer and octamethylcyclotetrasiloxane serving as raw materials to prepare a double-end hydroxyl POSS end-capped silicon-oxygen polymer.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
according to hydrosilylation reaction and chain extension reaction, a double-end hydroxyl POSS end-capped silicon-oxygen polymer and a single-end hydroxyl POSS end-capped silicon-oxygen polymer with different molecular chain lengths and different hydroxyl contents are designed and synthesized, the hydroxyl POSS end-capped silicon-oxygen polymer is used as a foaming auxiliary agent to prepare a foamed silicon rubber sealing sheet, and a test shows that the micro-morphological structure of the foamed silicon rubber sealing sheet is a circular cell structure with the average pore diameter distributed between 20 and 60 mu m, the cells are independently closed-cell distributed, the independent closed-cell structure with the average pore diameter distributed between 20 and 60 mu m endows the foamed silicon rubber sealing sheet with excellent mechanical properties, specifically, the compression stress required by 25% compression is increased to 121kPa, the compression permanent deformation CS (compression 50%,22h and 70 ℃) is between 3.8 and 4.2%, and the foamed silicon rubber sealing sheet is endowed with excellent sealing performance, and the specific expression is that the water absorption of the foamed silicon rubber sealing sheet is between 1.4 and 1.5%;
and the invention finds that: the foamed silicone rubber sealing sheet adopting the double-end hydroxyl POSS terminated silica-oxygen polymer as the foaming auxiliary agent is superior to the foamed silicone rubber sealing sheet adopting the single-end hydroxyl POSS terminated silica-oxygen polymer as the foaming auxiliary agent in the aspects of mechanical property and internal foam uniformity.
Detailed Description
A foamed silicone rubber sealing sheet is formed by punching a prepared foamed silicone rubber material through a cutting die, and the interior of the foamed silicone rubber sealing sheet comprises a circular cell structure with the average pore size distributed between 20 and 60 mu m, wherein the cells are independently closed-cell distributed;
wherein, the formula of the foaming silicon rubber material is as follows: 100phr of vinyl silicone oil with the viscosity of 8000 mPas, 6-20phr of foaming auxiliary agent, 0.5-1.5phr of platinum catalyst with the content of 1000PPM, 0.1-0.4phr of inhibitor and 25-60phr of hydrogen-containing silicone oil with the hydrogen content of 0.12 percent;
the foaming auxiliary agent is hydroxyl POSS terminated silica polymer, and the hydroxyl content of the foaming auxiliary agent is 3-7.7%;
the foaming silicon rubber sealing sheet has the compression stress required by 25% of compression of 90-120kPa, the compression permanent deformation CS (50% of compression, 22h,70 ℃) of 3.9-4.2% and the water absorption of 1.4-1.5%;
the hydroxyl POSS terminated silicone polymers described above include: the double-end hydroxyl POSS end-capped silica polymer and the single-end hydroxyl POSS end-capped silica polymer;
the synthesis method of the double-end hydroxyl POSS terminated silica polymer comprises the following steps:
step1-1, taking hydrogen-containing POSS (T8H 8), p-divinylbenzene and tetramethyldisiloxane as reaction monomers, and synthesizing a double-ended hydrosilation POSS end-capping siloxane functional monomer through a hydrosilylation reaction, wherein the specific synthesis steps are as follows: putting 720mg of hydrogen-containing POSS (T8H 8), 134mg of tetramethyldisiloxane and 100mL of toluene into a 500mL round-bottom four-neck flask with a magnetic stirrer, a burette, an argon inlet and a condenser, introducing argon for 30min, then adding 50mg of chloroplatinic acid, stirring and heating to 60 ℃, adding 260mg of p-divinylbenzene, reacting in a 60 ℃ oil bath at constant temperature for 1H, then heating to 100 ℃ for reacting at constant temperature for 8H, distilling under reduced pressure, and collecting fractions to obtain a double-end silicon-hydrogenated POSS end-capped functional monomer;
step1-2, synthesizing a double-end hydroxyl POSS terminated silica functional monomer by taking a double-end hydrosilation POSS terminated silica functional monomer and 4-hydroxystyrene as reaction monomers through a hydrosilylation reaction, wherein the specific synthesis steps are as follows: 557mg of double-ended hydrosilation POSS end-capped silica functional monomer and 100mL of toluene are placed into a 500mL round-bottom four-neck flask with a magnetic stirrer, a burette, an argon inlet and a condenser, argon is firstly introduced for 30min, then 60mg of chloroplatinic acid is added, the flask is stirred and heated to 80 ℃, 840mg of 4-hydroxystyrene is added, the flask is subjected to constant-temperature reaction in an oil bath at 80 ℃ for 2h, then the flask is heated to 110 ℃ and subjected to constant-temperature reaction for 10h, reduced-pressure distillation is carried out, and fractions are collected to obtain the double-ended hydroxyl POSS end-capped silica functional monomer;
step1-3, carrying out chain extension reaction on a double-end hydroxyl POSS terminated silica functional monomer and octamethylcyclotetrasiloxane serving as raw materials to prepare a double-end hydroxyl POSS terminated silica polymer, wherein the specific synthesis steps are as follows: putting a double-end hydroxyl POSS end-capped silica functional monomer and octamethylcyclotetrasiloxane into a 500mL round-bottom four-neck flask with a magnetic stirrer, a burette, a nitrogen inlet and a condenser, adding 50mg of a trifluoromethanesulfonic acid catalyst under the condition of introducing nitrogen, stirring and heating to 60 ℃ in an oil bath, reacting for 24 hours at constant temperature, distilling under reduced pressure, and collecting fractions to obtain a double-end hydroxyl POSS end-capped silica polymer;
699mg of double-end hydroxyl POSS end-capped silica functional monomer and 74mg of octamethylcyclotetrasiloxane are taken, and the double-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 D-1 The hydroxyl content thereof is 7.7%;
699mg of double-end hydroxyl POSS end-capped silica functional monomer and 444mg of octamethylcyclotetrasiloxane are taken, and the double-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 D-2 The hydroxyl content is 5.2%;
699mg of double-end hydroxyl POSS end-capped silica functional monomer and 740mg of octamethylcyclotetrasiloxane are taken, and the double-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 D-3 The hydroxyl content thereof is 4.1%;
the synthesis method of the single-end hydroxyl POSS end-capped silicone polymer comprises the following steps:
step2-1, taking 360mg of hydrogen-containing POSS (T8H 8), 130mg of p-divinylbenzene and 134mg of tetramethyldisiloxane as reaction monomers, and synthesizing a single-end type hydrosilation POSS end-capped silica functional monomer through a hydrosilylation reaction according to the synthesis steps in the Step 1-1;
step2-2, synthesizing a single-end type hydroxyl POSS end-capped silicon-oxygen functional monomer by taking 312mg of single-end type hydrosilation POSS end-capped silicon-oxygen functional monomer and 480mg of 4-hydroxystyrene as reaction monomers through hydrosilylation reaction according to the synthesis Step in the Step 1-2;
step2-3, carrying out chain extension reaction on a single-end hydroxyl POSS end-capped silicon-oxygen functional monomer and octamethylcyclotetrasiloxane serving as raw materials to prepare a single-end hydroxyl POSS end-capped silicon-oxygen polymer;
396mg of single-end hydroxyl POSS end-capped silica functional monomer and 74mg of octamethylcyclotetrasiloxane are taken, and the single-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 S-1 The hydroxyl content is 7.2%;
396mg of single-end hydroxyl POSS end-capped silica functional monomer and 444mg of octamethylcyclotetrasiloxane are taken, and the single-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 S-2 The hydroxyl content is 4.0%;
396mg of single-end hydroxyl POSS end-capped silica functional monomer and 740mg of octamethylcyclotetrasiloxane are taken, and the single-end hydroxyl POSS end-capped silica polymer P is prepared according to the synthesis steps in the Step1-3 S-3 The hydroxyl content is 3.0%;
example 1: terminated siloxane polymer P with double-ended hydroxyl POSS D-1 For the foaming aid, a foamed silicone rubber sealing sheet S was prepared D-1 The preparation method comprises the following specific steps:
step I, preparing a component I containing a catalyst, wherein the component I comprises the following raw materials: 50phr vinyl silicone oil (viscosity 8000 mPa.s), foaming auxiliary agent-double-end type hydroxyl POSS end-capped silicon-oxygen polymer P D-1 15phr, 0.8phr (content 1000 PPM) of platinum catalyst and 0.2phr of inhibitor-methylbutinol, and the raw materials are uniformly dispersed by a homogenizer and then are stored for standby;
step II, preparing a component II containing a cross-linking agent, wherein the component II comprises the following raw materials in formula: 50phr of vinyl silicone oil (the viscosity is 8000 mPa.s) and 45phr of cross-linking agent-hydrogen-containing silicone oil (the hydrogen content is 0.12 percent), and the raw materials are uniformly dispersed by a homogenizer and then are stored for standby;
step III, preparing the component I and the component II according to the mass ratio of 1 to 1, then shearing and mixing the raw material components uniformly at a high speed by using a dispersion machine, vacuumizing to remove bubbles, pouring into a tetrafluoroethylene-plated steel mould, adding a cover plate, vulcanizing at room temperature for 1 hour, and then vulcanizing at 100 ℃ for 1 hour for the second time to obtain a foamed silicone rubber material;
step IV, placing the vulcanized foamed silicone rubber material into a 100 ℃ oven for constant temperature treatment for 12h, and then punching the material into a foamed silicone rubber sealing sheet S through a cutting die D-1 The width of the plate is 602mm, and the thickness of the plate is 5.03mm;
to the foamed silicone rubber sealing sheet S D-1 The following performance tests were performed:
(1) The foamed silicon rubber sealing sheet is brittle-broken by adopting liquid nitrogen, and after the section is subjected to vacuum metal spraying treatment, the microscopic morphological structure of the foamed silicon rubber sealing sheet is observed by adopting a scanning electron microscope as follows: the distribution is uniform, the average pore diameter of the cells is 40 mu m, most cells are in independent closed circular structures, and part of cells are fused;
(2) According to GB/T6343-2009 'determination of apparent density of foam and rubber', the apparent density of the foamed silicone rubber sealing sheet is determined to be 0.42g/cm 3 ；
(3) According to GB/T6344-2008 'determination of tensile strength and elongation at break of flexible foam polymer material', the tensile strength of the foamed silicone rubber sealing sheet is determined to be 0.57MPa, and the elongation at break is determined to be 103%;
(4) According to GB/T7757-2009 determination of compression stress strain performance of vulcanized rubber or thermoplastic rubber, the required compression stress of 25% of the foamed silicone rubber sealing sheet is determined to be 112kPa;
(5) The water absorption of the foamed silicone rubber seal sheet was determined to be 1.42% according to the method specified in ASTM D1056 "standard for tough porous materials-sponge or expanded rubber";
(6) According to GB/T6669-2008 'determination of compression set of flexible foam polymer material', the compression set CS (compression 50%,22h,70 ℃) of the foamed silicone rubber sealing sheet is determined to be 4.07%;
(7) According to the method A specified in GB/T1685-2008 'determination of compression stress relaxation of vulcanized rubber or thermoplastic rubber at normal temperature and high temperature', the compression stress relaxation performance of the foamed silicone rubber sealing sheet material at the accelerated aging of 85 ℃/2000h is determined, and the stress relaxation is 13.9%;
single-ended hydroxyl POSS terminated siloxane polymer P S-1 Preparing a foaming silicone rubber sealing sheet S as a foaming auxiliary agent according to the steps of Step I, step II, step III and Step IV S-1 603mm in width and 4.97mm in thickness, and tested, the foamed silicone rubber sealing sheet S S-1 The microstructure of (A) is a circular structure with independent closed cell distribution and average pore size distribution between 30 and 60 mu m, a few cell fusion phenomena exist, and the apparent density of the microstructure is 0.39g/cm 3 0.52MPa tensile strength, 117% elongation at break, 105kPa compressive stress required for 25% compression, 1.40% water absorption, and 4.19% compression set CS (50% compression, 22h,70 ℃ C.);
example 2: end capping of siloxane polymers P with double-ended hydroxyl POSS D-2 For the foaming aid, a foamed silicone rubber sealing sheet S was prepared D-2 The preparation method comprises the following specific steps:
step I, preparing a component I containing a catalyst, wherein the component I comprises the following raw materials: 50phr vinyl silicone oil (viscosity 8000 mPa.s), foaming auxiliary agent-double-end type hydroxyl POSS end-capped silicon-oxygen polymer P D-2 6phr of platinum catalyst, 1.5phr (content: 1000 PPM) of platinum catalyst and 0.4phr of inhibitor-methylbutinol, and the raw materials are uniformly dispersed by a homogenizer and then are stored for standby;
step II, preparing a component II containing a cross-linking agent, wherein the component II comprises the following raw materials in formula: 50phr (viscosity 8000mPa & s) of vinyl silicone oil and 60phr (hydrogen content of 0.12%) of cross-linking agent-hydrogen-containing silicone oil, and the raw materials are uniformly dispersed by a homogenizer and then are stored for later use;
step III, preparing the component I and the component II according to the mass ratio of 1 to 1, then shearing and mixing the raw material components uniformly at a high speed by using a dispersion machine, vacuumizing to remove bubbles, pouring into a tetrafluoroethylene-plated steel mould, adding a cover plate, vulcanizing at room temperature for 0.5h, and then vulcanizing twice at 80 ℃ for 2.5h to obtain a foamed silicone rubber material;
step IV, placing the vulcanized foamed silicone rubber material into a 80 ℃ oven for constant temperature treatment for 15h, and then punching the material into a foamed silicone rubber sealing sheet S with the width of 600mm and the thickness of 5mm by a cutting die D-2 601mm in width and 5.01mm in thickness, and tested, the foamed silicone rubber sealing sheet S D-2 The microscopic morphological structure of the nano-composite material is a cellular structure with uniform distribution and average pore diameter of 30 mu m, the cells are independent closed circular structures, the phenomenon of cell fusion hardly exists, and the apparent density is 0.51g/cm 3 0.50MPa tensile strength, 118% elongation at break, 94kPa compressive stress required for 25% compression, 1.48% water absorption, and 4.11% compression set CS (50% compression, 22h,70 ℃ C.);
single-end hydroxyl POSS end-capped silicon-oxygen polymer P S-2 Preparing a foaming silicone rubber sealing sheet S as a foaming auxiliary agent according to the steps of Step I, step II, step III and Step IV S-2 603mm in width and 5.00mm in thickness, and tested, the foamed silicone rubber sealing sheet S S-2 The microstructure of (A) is a circular structure with independent closed pore distribution and average pore diameter distribution between 20 and 50 mu m, almost has no cell fusion phenomenon, and has apparent density of 0.45g/cm 3 0.47MPa tensile strength, 125% elongation at break, 91kPa compressive stress required for 25% compression, 1.51% water absorption, and 4.22% compression set CS (50% compression, 22h,70 ℃ C.);
example 3: terminated siloxane polymer P with double-ended hydroxyl POSS D-3 For the foaming aid, a foamed silicone rubber sealing sheet S was prepared D-3 The preparation method comprises the following specific steps:
step I, preparing a component I containing a catalyst, wherein the component I comprises the following raw materials in formula: 50phr vinyl silicone oil (viscosity 8000 mPa.s), foaming auxiliary agent-double-end type hydroxyl POSS end-capped silicon-oxygen polymer P D-3 20phr of platinum catalyst, 0.5phr (content: 1000 PPM) of platinum catalyst and 0.1phr of inhibitor-methylbutynol, and the raw materials are uniformly dispersed by a homogenizer and then storedStandby;
step II, preparing a component II containing a cross-linking agent, wherein the component II comprises the following raw materials in formula: 50phr of vinyl silicone oil (the viscosity is 8000 mPa.s) and 25phr of cross-linking agent-hydrogen-containing silicone oil (the hydrogen content is 0.12 percent), and the raw materials are uniformly dispersed by a homogenizer and then are stored for standby;
step III, preparing the component I and the component II according to the mass ratio of 1 to 1, then shearing and mixing the raw material components uniformly at a high speed by using a dispersion machine, vacuumizing to remove bubbles, pouring into a tetrafluoroethylene-plated steel mould, adding a cover plate, vulcanizing at room temperature for 2 hours, and then vulcanizing at 90 ℃ for 2 hours for the second time to obtain a foamed silicone rubber material;
step IV, placing the vulcanized foamed silicone rubber material into a 100 ℃ oven for constant temperature treatment for 12h, and punching the material into a foamed silicone rubber sealing sheet S with the width of 600mm and the thickness of 5mm by a cutting die D-3 The foamed silicone rubber sealing sheet S was tested to have a width of 600mm and a thickness of 5.01mm D-3 The microstructure of the composite material is a cellular structure with uniform distribution and average pore diameter of 40 mu m, the cells are independent closed circular structures, the phenomenon of fusion of a few cells exists, and the apparent density is 0.43g/cm 3 A tensile strength of 0.68MPa, an elongation at break of 102%, a compressive stress required for 25% compression of 121kPa, a water absorption of 1.40%, and a compression set CS (50% compression, 22h,70 ℃) of 3.87%;
single-end hydroxyl POSS end-capped silicon-oxygen polymer P S-3 Preparing a foaming silicone rubber sealing sheet S as a foaming auxiliary agent according to the steps of Step I, step II, step III and Step IV S-3 603mm in width and 5.02mm in thickness, and tested, the foamed silicone rubber sealing sheet S S-3 The microstructure of (A) is a circular structure with independent closed pore distribution and average pore size distribution between 30 and 50 mu m, almost has no cell fusion phenomenon, and has an apparent density of 0.41g/cm 3 A tensile strength of 0.61MPa, an elongation at break of 114%, a compressive stress required for 25% compression of 110kPa, a water absorption of 1.37%, and a compression set CS (50% compression, 22h,70 ℃) of 3.94%;
as can be seen from the test data in examples 1 to 3, the mechanical properties of the foamed silicone rubber sealing sheet adopting the double-ended hydroxyl POSS terminated siloxane polymer as the foaming auxiliary agent are superior to those of the foamed silicone rubber sealing sheet adopting the single-ended hydroxyl POSS terminated siloxane polymer as the foaming auxiliary agent, and the difference between the water absorption properties of the foamed silicone rubber sealing sheet and the water absorption properties of the foamed silicone rubber sealing sheet is not large;
since the hydroxyl activity at both ends of the single-ended hydroxyl POSS terminated siloxane polymer is different, H is released during foaming 2 The rate of (b) is different, so that the pore size distribution range of the cells of the foamed silicone rubber sealing sheet using the same as a foaming auxiliary agent is wider; the hydroxyl activity at two ends of the double-end hydroxyl POSS terminated siloxane polymer is equivalent, so that H is released during foaming 2 The rate of the foaming agent is basically not greatly different, so that the foamed silicone rubber sealing sheet taking the foaming agent as a foaming auxiliary agent has more uniform cell structure and smaller pore size distribution range of cells.
Claims (5)
1. A foamed silicone rubber sealing sheet is characterized in that the foamed silicone rubber sealing sheet is formed by punching a prepared foamed silicone rubber material through a cutting die, the interior of the foamed silicone rubber sealing sheet comprises a circular cell structure with the average pore diameter distributed between 20 and 60 mu m, and the cells are independently distributed with closed cells;
wherein, the formula of the foaming silicon rubber material is as follows: 100phr of vinyl silicone oil with the viscosity of 8000 mPas, 6-20phr of foaming auxiliary agent, 0.5-1.5phr of platinum catalyst with the content of 1000PPM, 0.1-0.4phr of inhibitor and 25-60phr of hydrogen-containing silicone oil with the hydrogen content of 0.12 percent;
the foaming auxiliary agent is hydroxyl POSS terminated silica polymer, and the hydroxyl content of the foaming auxiliary agent is 3-7.7%;
the synthesis method of the hydroxyl POSS terminated siloxane polymer comprises the following steps:
step1-1, taking hydrogen-containing POSS, p-divinylbenzene and tetramethyl disiloxane as reaction monomers, and synthesizing a silicon-oxygen functional monomer terminated by hydrosilation POSS through hydrosilylation reaction;
step1-2, taking a hydrosilylation POSS terminated silica functional monomer and 4-hydroxystyrene as reaction monomers, and synthesizing a hydroxyl POSS terminated silica functional monomer through hydrosilylation reaction;
step1-3, taking a hydroxyl POSS terminated silica functional monomer and octamethylcyclotetrasiloxane as raw materials to carry out chain extension reaction to prepare the hydroxyl POSS terminated silica polymer.
2. The foamed silicone rubber sealing sheet according to claim 1, wherein the foamed silicone rubber sealing sheet has a compressive stress of 90 to 120kPa required for 25% compression, a compression set CS of 3.9 to 4.2%, and a water absorption of 1.4 to 1.5%; the test parameters for the compression set CS were 50% compression, 22h,70 ℃.
3. The foamed silicone rubber sealing sheet according to claim 1, wherein the foamed silicone rubber sealing sheet is prepared by the steps of:
step I, preparing a component I containing a catalyst, wherein the component I comprises the following raw materials in formula: vinyl silicone oil, a foaming auxiliary agent, a platinum catalyst and an inhibitor, wherein the raw materials are uniformly dispersed by a homogenizer and then are stored for later use;
step II, preparing a component II containing a cross-linking agent, wherein the component II comprises the following raw materials in formula: vinyl silicone oil and cross-linking agent-hydrogen-containing silicone oil, wherein the raw materials are uniformly dispersed by a homogenizer and then are stored for later use;
step III, preparing the component I and the component II according to the mass ratio of 1;
and Step IV, placing the vulcanized foaming silicone rubber material into an oven at the temperature of 80-100 ℃ for constant temperature treatment for 12-15h, and punching the material into a foaming silicone rubber sealing sheet with the width of (600-605) mm and the thickness of (5 +/-0.3) mm by using a cutting die.
4. The foamed silicone rubber sealing sheet according to claim 1, wherein the foaming auxiliary is a double-ended hydroxyl POSS-terminated silicone polymer or a single-ended hydroxyl POSS-terminated silicone polymer.
5. The foamed silicone rubber sealing sheet according to claim 1, wherein the hydrogen-containing POSS is T8H8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211116016.XA CN115216156B (en) | 2022-09-14 | 2022-09-14 | Foamed silicone rubber sealing sheet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211116016.XA CN115216156B (en) | 2022-09-14 | 2022-09-14 | Foamed silicone rubber sealing sheet and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115216156A CN115216156A (en) | 2022-10-21 |
| CN115216156B true CN115216156B (en) | 2022-12-09 |
Family
ID=83616830
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211116016.XA Active CN115216156B (en) | 2022-09-14 | 2022-09-14 | Foamed silicone rubber sealing sheet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115216156B (en) |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2773166B1 (en) * | 1997-12-31 | 2000-03-24 | Rhodia Chimie Sa | AQUEOUS SILICONE EMULSION, USEFUL AS A BASE FOR THE PREPARATION OF WATER-REPELLENT COATING AND ANTI-ADHESIVE FOR PAPER, METHOD FOR PREPARING AN EMULSION OF THIS TYPE AND ANTI-ADHERENT COATINGS |
| CN103849150B (en) * | 2014-02-24 | 2016-10-26 | 四川大学 | A kind of preparation method of POSS modified polyorganosiloxane rubber composite |
| CN105647189B (en) * | 2016-01-29 | 2018-11-02 | 浙江凌志新材料有限公司 | A kind of organic foamed silastic |
| CN106633918B (en) * | 2017-01-13 | 2020-11-03 | 山东船舶技术研究院 | High-strength high-heat-resistance flame-retardant silicone rubber material and preparation method thereof |
| CN106750308A (en) * | 2017-02-09 | 2017-05-31 | 南京大学 | A kind of multi-hydroxy alkyl phenyl sesquisiloxane and its preparation method and purposes |
| CN110305368B (en) * | 2019-06-20 | 2021-03-26 | 杭州师范大学 | Flame-retardant foaming agent and preparation method and application thereof |
| CN111454455B (en) * | 2020-03-30 | 2022-04-12 | 江苏师范大学 | Porous hybrid polymer rich in POSS (polyhedral oligomeric silsesquioxane) derived silicon hydroxyl and preparation method and catalytic application thereof |
| WO2022000413A1 (en) * | 2020-07-02 | 2022-01-06 | Wacker Chemie Ag | Foamable silicone composition |
| CN113956667B (en) * | 2021-10-22 | 2023-04-07 | 东莞市曦晨启明新材料科技有限公司 | Foaming silicone rubber and preparation method and application thereof |
-
2022
- 2022-09-14 CN CN202211116016.XA patent/CN115216156B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN115216156A (en) | 2022-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100961638B1 (en) | High Fracture Toughness Hydrosilylation Cured Silicone Resin | |
| CN107353871B (en) | High-temperature-resistant bonding sealing silicone resin and preparation method thereof | |
| KR100701549B1 (en) | Proton conducting film, method for producing the same, and fuel cell using the same | |
| Fang et al. | Thermal degradation mechanism of addition-cure liquid silicone rubber with urea-containing silane | |
| Rao et al. | Preparation and oxygen/nitrogen permeability of PDMS crosslinked membrane and PDMS/tetraethoxysilicone hybrid membrane | |
| EP3279246B1 (en) | Porous body, and method for producing porous body | |
| Isayeva et al. | Amphiphilic membranes crosslinked and reinforced by POSS | |
| CN102181056B (en) | Copolymerized high-performance damping silicon rubber and preparation method thereof | |
| CN102827371A (en) | Functional polysiloxane, preparation method of functional polysiloxane and application of functional polysiloxane in gas separation membrane | |
| SK902000A3 (en) | New block copolymers and preparation thereof | |
| Yang et al. | A review of poly [(3, 3, 3-trifluoropropyl) methylsiloxane]: Synthesis, properties and applications | |
| Song et al. | Preparation and characterization of epoxy resin modified with alkoxysilane‐functionalized poly (urethane‐imide) by the sol–gel process | |
| CN115216156B (en) | Foamed silicone rubber sealing sheet and preparation method thereof | |
| CN103834354A (en) | Preparation of an organosilicone pressure-sensitive adhesive and applications of the organosilicone pressure-sensitive adhesive | |
| CN111183009A (en) | Curable organopolysiloxane compositions containing dynamic covalent polysiloxanes | |
| CN112920423B (en) | Preparation method of core-shell structure organic silicon resin | |
| CN110591377A (en) | Preparation method and application of transparent epoxy resin-silicon rubber modified material | |
| CN117083347A (en) | Addition reaction curable organopolysiloxane composition | |
| US20240150527A1 (en) | Liquid vinyl functionalized cage-type polyhedral oligomeric silsesquioxane modified by low-molecular-weight polysiloxane and preparation method thereof | |
| Zeng et al. | Synthesis and application of adhesion promoter containing phenolic hydroxyl/acrylate groups for addition-cure liquid silicone rubber | |
| KR102131611B1 (en) | Formulations containing metal aprotic organosilane oxide compounds | |
| CN112795198A (en) | High-flame-retardant organic silicon foam sheet and preparation method thereof | |
| CN109096775A (en) | A kind of super-low-hardness dual composition addition type liquid silastic and preparation method thereof | |
| CN115304920A (en) | Organic silicon foaming material and preparation method and application thereof | |
| CN111484620B (en) | Adhesion promoter for addition type silicone rubber, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |