CN113930076A - Organosilicon foam material, preparation method and application - Google Patents

Organosilicon foam material, preparation method and application Download PDF

Info

Publication number
CN113930076A
CN113930076A CN202111149944.1A CN202111149944A CN113930076A CN 113930076 A CN113930076 A CN 113930076A CN 202111149944 A CN202111149944 A CN 202111149944A CN 113930076 A CN113930076 A CN 113930076A
Authority
CN
China
Prior art keywords
parts
silicone oil
component
foam
aluminum hydroxide
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.)
Pending
Application number
CN202111149944.1A
Other languages
Chinese (zh)
Inventor
段玉兵
李鹏飞
姚金霞
张皓
马国庆
胡晓黎
贾然
陈子龙
李程启
林颖
刘嵘
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
Original Assignee
State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by State Grid Corp of China SGCC, Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd filed Critical State Grid Corp of China SGCC
Priority to CN202111149944.1A priority Critical patent/CN113930076A/en
Publication of CN113930076A publication Critical patent/CN113930076A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/02Working-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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066Use of inorganic compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066Use of inorganic compounding ingredients
    • C08J9/0071Nanosized fillers, i.e. having at least one dimension below 100 nanometers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00Characterised 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
    • C08J2383/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • C08J2483/05Polysiloxanes containing silicon bound to hydrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • C08J2483/08Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides an organosilicon foam material, which comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1: 1-1: 2, and the component A comprises the following components in parts by weight: 100 parts of hydroxyl silicone oil, 10-40 parts of aluminum hydroxide, 2-20 parts of flaky filler, 5-10 parts of nano calcium carbonate and 1-3 parts of catalyst; the component B comprises the following components in parts by weight: 80-90 parts of hydroxyl silicone oil, 10-20 parts of isocyanate terminated silicone oil, 10-40 parts of aluminum hydroxide, 5-10 parts of fumed silica, 1-3 parts of inhibitor and 2-15 parts of hydrogen-containing silicone oil. The invention also provides a preparation method and application of the organic silicon foam material. The flaky filler, the aluminum hydroxide and the nano calcium carbonate have a synergistic effect, so that the fireproof performance is better; the isocyanate group of the isocyanate-terminated silicone oil reacts with hydroxyl, Si-H, carbamate group and the like in the system to form a cross-linking structure, and the polar functional group is introduced to improve the strength of the material.

Description

Organosilicon foam material, preparation method and application
Technical Field
The invention relates to the technical field of high polymer material research and processing, in particular to an organic silicon foam material, a preparation method and application.
Background
The room temperature vulcanized silicone rubber foam material is a polymer foam material which is formed by condensation, dehydrogenation and foaming under the action of a catalyst by taking hydroxy-terminated polydimethylsiloxane as a base rubber and hydrogen-containing silicone oil as a cross-linking agent. The high polymer foam material not only has the advantages of high and low temperature resistance, irradiation resistance, aging resistance, corrosion resistance, physiological inertia, excellent electrical insulation and the like of the silicon rubber, but also has the excellent characteristics of light weight, softness, sound and heat insulation, impact resistance and the like of the foam material, and is widely applied to the fields of national defense, electric power, electronics, aerospace, transportation and the like.
As a fire-proof blocking material, a relatively complete structure needs to be kept in the fire, so that the spread of the fire is blocked. However, the existing flame-retardant organic silicon foam material mainly realizes the flame-retardant property by adding a large amount of flame-retardant additives, and the defect of the mode is that the prepared material is easy to deform and crack in flame and is difficult to have the fireproof blocking effect of blocking the flame. The silicon rubber foam has low strength and rigidity, low foaming multiplying power and high foam density, and limits the application of the silicon rubber foam.
Disclosure of Invention
The invention provides an organosilicon foam material, a preparation method and application, solves the problem that the organosilicon foam material is easy to deform and crack in flame in the prior art, and simultaneously improves the foam strength.
The technical scheme of the invention is realized as follows:
according to a first aspect of embodiments of the present invention, there is provided a silicone foam.
In one embodiment, the silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1: 1-1: 2, wherein,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil, 10-40 parts of aluminum hydroxide, 2-20 parts of flaky filler, 5-10 parts of nano calcium carbonate and 1-3 parts of catalyst;
the component B comprises the following raw material components in parts by weight:
80-90 parts of hydroxyl silicone oil, 10-20 parts of isocyanate terminated silicone oil, 10-40 parts of aluminum hydroxide, 5-10 parts of fumed silica, 1-3 parts of inhibitor and 2-15 parts of hydrogen-containing silicone oil.
Optionally, the organosilicon foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1: 1-1: 2, wherein,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil, 25 parts of aluminum hydroxide, 20 parts of flaky filler, 5 parts of nano calcium carbonate and 1.5 parts of catalyst;
the component B comprises the following raw material components in parts by weight:
85 parts of hydroxyl silicone oil, 15 parts of isocyanate-terminated silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of inhibitor and 9 parts of hydrogen-containing silicone oil.
Optionally, the plate-like filler is one or more of molybdenum dioxide, graphene and mica.
Optionally, the viscosity of the hydroxyl silicone oil is 500-20000 mPa.s.
Optionally, the catalyst is a platinum catalyst, and the platinum content is 500-5000 ppm.
Optionally, the inhibitor is an alkynol or phenylacetylene, which acts to adjust the curing time or working time.
Optionally, the preparation method of the isocyanate-terminated silicone oil comprises the following steps:
reacting diisocyanate and alpha, omega-dihydroxypropyl terminated silicone oil for 6 hours at room temperature under the catalysis of dibutyltin dilaurate, wherein the molar ratio of the diisocyanate to the alpha, omega-dihydroxypropyl terminated silicone oil is 1:1.
Alternatively, the dibutyltin dilaurate is added in an amount of 1% of the total mass of the diisocyanate and the alpha, omega-dihydroxypropyl terminated silicone oil.
Optionally, the diisocyanate is toluene diisocyanate TDI or hexamethylene diisocyanate HDI.
Optionally, the hydrogen content of the hydrogen-containing silicone oil is 0.5% to 1.4%.
According to a second aspect of embodiments of the present invention, there is provided a method of preparing a silicone foam for preparing the silicone foam of the above embodiments.
In one embodiment, a method of making a silicone foam includes the steps of:
stirring hydroxyl silicone oil, aluminum hydroxide, flaky filler and nano calcium carbonate to obtain a mixed solution 1;
grinding the mixed solution 1, adding a catalyst, and uniformly mixing to obtain a component A; firstly, the filler with large dosage is uniformly mixed to obtain a mixed solution 1, and then the catalyst is added, so that the loss of the catalyst or the generation of side reaction can be avoided;
stirring hydroxyl silicone oil, isocyanate-terminated silicone oil, aluminum hydroxide, fumed silica, an inhibitor and hydrogen-containing silicone oil to obtain a mixed solution 2;
grinding the mixed solution 2 to obtain a component B;
and (5) mixing and stirring the prepared component A and the prepared component B uniformly to prepare the organic silicon foam material.
In the above examples, the steps of preparing component A in steps (1) and (2) and the steps of preparing component B in steps (3) and (4) may be reversed in order of preparation of component A and component B.
Optionally, in the step (1) and the step (3), the stirring speed is 1000-1500 r/min, and the stirring time is 30-50 min.
Optionally, in the step (2) and the step (4), the grinding rotating speed is 80-100 r/min.
Optionally, in the step (2) and the step (4), the grinding time is 1-2 hours.
Optionally, in the step (2) and the step (4), grinding is completed by using a three-roll grinding machine.
According to a third aspect of embodiments of the present invention there is provided a use of a silicone foam, in one embodiment, for fire blocking of electrical power construction equipment.
According to a fourth aspect of embodiments of the present invention, there is provided a use of a silicone foam, in one embodiment, for a new energy battery foam barrier layer.
According to a fifth aspect of embodiments of the present invention, there is provided a use of a silicone foam, in one embodiment, the silicone foam is used for a chemical equipment insulation layer.
The invention has the beneficial effects that:
the component A comprises the flaky filler, the flaky filler has large specific surface area, good thermal stability and chemical stability, can easily form a continuous and compact inorganic shell structure with other powdery fillers in flame, is not easy to crack in the ablation process, and can play a good role in blocking; the aluminum hydroxide has a flame retardant effect, and the nano calcium carbonate has a stabilizing effect of preventing deformation, so that the flaky filler, the aluminum hydroxide and the nano calcium carbonate have a synergistic effect to form better fireproof performance. The component B comprises the isocyanate-terminated silicone oil, so that the problem of phase separation caused by the reaction of directly adding isocyanate and the hydroxypropyl-terminated silicone oil or the hydroxyl silicone oil is avoided, the isocyanate group can react with active hydrogen-containing groups such as hydroxyl, Si-H, carbamate and the like in a system to form more cross-linked structures, and polar functional groups are introduced, so that the intermolecular force is increased, and the strength of the organic silicon foam is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a photograph of example 1 of the present invention after ablation;
FIG. 2 is a photograph of example 2 of the present invention after ablation;
FIG. 3 is a photograph of the ablated material of example 3 of the present invention;
FIG. 4 is a photograph of the ablated material of example 4 of the present invention;
FIG. 5 is a photograph of example 5 of the present invention after ablation;
FIG. 6 is a photograph of comparative example 1 of the present invention after ablation;
FIG. 7 is a photograph of comparative example 2 of the present invention after ablation.
Detailed Description
To make the features and effects of the present invention comprehensible to those having ordinary knowledge in the art, general description and definitions are made with respect to terms and phrases mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In this document, the terms "comprising," "including," "having," "containing," or any other similar term, are intended to be open-ended franslational phrase (open-ended franslational phrase) and are intended to cover non-exclusive inclusions. For example, a composition or article comprising a plurality of elements is not limited to only those elements recited herein, but may include other elements not expressly listed but generally inherent to such composition or article. In addition, unless expressly stated to the contrary, the term "or" is intended to mean an inclusive "or" rather than an exclusive "or". For example, the condition "a or B" is satisfied in any of the following cases: a is true (or present) and B is false (or not present), a is false (or not present) and B is true (or present), both a and B are true (or present). Furthermore, in this document, the terms "comprising," including, "" having, "" containing, "and" containing "are to be construed as specifically disclosed and to cover both closed and semi-closed conjunctions, such as" consisting of … "and" consisting essentially of ….
All features or conditions defined herein as numerical ranges or percentage ranges are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to have covered and specifically disclosed all possible subranges and individual numerical values within the ranges, particularly integer numerical values. For example, a description of a range of "1 to 8" should be considered to have specifically disclosed all subranges such as 1 to 7, 2 to 8, 2 to 6, 3 to 6, 4 to 8, 3 to 8, and so on, particularly subranges bounded by all integer values, and should be considered to have specifically disclosed individual values such as 1, 2, 3, 4, 5, 6, 7, 8, and so on, within the range. Unless otherwise indicated, the foregoing explanatory methods apply to all matters contained in the entire disclosure, whether broad or not.
If an amount or other value or parameter is expressed as a range, preferred range, or a list of upper and lower limits, it is to be understood that all ranges subsumed therein for any pair of that range's upper or preferred value and that range's lower or preferred value, whether or not such ranges are separately disclosed, are specifically disclosed herein. Further, when a range of numerical values is recited herein, unless otherwise stated, the range is intended to include the endpoints thereof, and all integers and fractions within the range.
In this context, numerical values should be understood to have the precision of the number of significant digits of the value, provided that the object of the invention is achieved. For example, the number 40.0 should be understood to cover a range from 39.50 to 40.49. In this document, where Markush group (Markush group) or Option language is used to describe features or examples of the invention, those skilled in the art will recognize that a sub-group of all elements or any individual element within a Markush group or list of options may also be used to describe the invention. For example, if X is described as "selected from the group consisting of1、X2And X3The group "also indicates that X has been fully described as X1Is claimed with X1And/or X2Claim (5). Furthermore, where Markush group or option terms are used to describe features or examples of the invention, those skilled in the art will recognize that any combination of sub-groups of all elements or individual elements within the Markush group or option list can also be used to describe the invention. Accordingly, for example, if X is described as "selected from the group consisting of1、X2And X3Group consisting of "and Y is described as" selected from Y1、Y2And Y3The group "formed indicates that X has been fully described as X1Or X2Or X3And Y is Y1Or Y2Or Y3Claim (5).
The following detailed description is merely exemplary in nature and is not intended to limit the invention or the application thereof. Furthermore, there is no intention to be bound by any theory presented in the preceding prior art or the summary of the invention or the following detailed description or examples.
Example 1
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000 mPas, 40 parts of aluminum hydroxide, 3 parts of graphene, 10 parts of nano calcium carbonate and 1.5 parts of platinum catalyst with platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
85 parts of hydroxyl silicone oil with the viscosity of 500 mPas, 15 parts of TDI end-blocked silicone oil, 30 parts of aluminum hydroxide, 3 parts of fumed silica, 1 part of alkynol and 15 parts of hydrogen-containing silicone oil with the hydrogen content of 0.8 percent (wt percent).
Optionally, the preparation method of the TDI terminated silicone oil comprises the following steps:
and reacting TDI and alpha, omega-dihydroxypropyl terminated silicone oil for 6 hours at room temperature under the catalysis of dibutyltin dilaurate, wherein the molar ratio of TDI to alpha, omega-dihydroxypropyl terminated silicone oil is 1:1.
Alternatively, the amount of dibutyltin dilaurate added is 1% of the total mass of TDI and α, ω -dihydroxypropyl terminated silicone oil.
The preparation method of the organic silicon foam material comprises the following steps:
(1) hydroxyl silicone oil, aluminum hydroxide, flaky filler and nano calcium carbonate are stirred for 50min at the speed of 1000r/min to obtain a mixed solution 1;
(2) grinding the mixed solution 1 on a three-roll grinder for 2 hours at a rotating speed of 80r/min, and then adding a catalyst to mix uniformly to obtain a component A;
(3) stirring hydroxyl silicone oil, isocyanate-terminated silicone oil, aluminum hydroxide, fumed silica, an inhibitor and hydrogen-containing silicone oil to obtain a mixed solution 2;
(4) grinding the mixed solution 2 on a three-roll grinder for 2 hours at a rotating speed of 80r/min to obtain a component B;
(5) and (3) uniformly mixing and stirring the prepared component A and the prepared component B to prepare the organic silicon foam material.
Example 2
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000 mPas, 25 parts of aluminum hydroxide, 20 parts of mica, 5 parts of nano calcium carbonate and 1.5 parts of platinum catalyst with platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
85 parts of hydroxyl silicone oil with the viscosity of 500 mPas, 15 parts of TDI end-capped silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of alkynol and 9 parts of hydrogen-containing silicone oil with the hydrogen content of 0.8 percent (wt%).
The preparation method of the organic silicon foam material comprises the following steps:
(1) hydroxyl silicone oil, aluminum hydroxide, flaky filler and nano calcium carbonate are stirred at the speed of 1500r/min for 30min to obtain a mixed solution 1;
(2) grinding the mixed solution 1 on a three-roll grinder for 1 hour at the rotating speed of 100r/min, and then adding a catalyst to be uniformly mixed to obtain a component A;
(3) stirring hydroxyl silicone oil, isocyanate-terminated silicone oil, aluminum hydroxide, fumed silica, an inhibitor and hydrogen-containing silicone oil to obtain a mixed solution 2;
(4) grinding the mixed solution 2 on a three-roll grinder for 1 hour at the rotating speed of 100r/min to obtain a component B;
(5) and (3) uniformly mixing and stirring the prepared component A and the prepared component B to prepare the organic silicon foam material.
Example 3
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1.5,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000 mPas, 25 parts of aluminum hydroxide, 10 parts of mica, 5 parts of nano calcium carbonate and 1.5 parts of platinum catalyst with platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
80 parts of hydroxyl silicone oil with the viscosity of 500 mPa.s, 20 parts of TDI end-capped silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of alkynol and 9 parts of hydrogen-containing silicone oil with the hydrogen content of 0.8 percent (wt percent).
The preparation method is the same as example 1.
Example 4
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000 mPas, 25 parts of aluminum hydroxide, 20 parts of mica, 10 parts of nano calcium carbonate and 3 parts of platinum catalyst with platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
80 parts of hydroxyl silicone oil with the viscosity of 500 mPas, 20 parts of HDI end-capped silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of alkynol and 5 parts of hydrogen-containing silicone oil with the hydrogen content of 1.4 percent (wt%).
Optionally, the preparation method of the HDI-terminated silicone oil comprises the following steps:
and (3) reacting HDI and alpha, omega-dihydroxypropyl terminated silicone oil for 6 hours at room temperature under the catalytic action of dibutyltin dilaurate, wherein the molar ratio of HDI to alpha, omega-dihydroxypropyl terminated silicone oil is 1:1.
Optionally, the addition amount of the dibutyltin dilaurate is 1% of the total mass of the HDI and the alpha, omega-dihydroxypropyl terminated silicone oil.
The preparation method is the same as example 1.
Example 5
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with the viscosity of 500 mPas, 25 parts of aluminum hydroxide, 20 parts of mica, 5 parts of nano calcium carbonate and 1.5 parts of platinum catalyst with the platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
85 parts of hydroxyl silicone oil with the viscosity of 500 mPas, 15 parts of TDI end-blocked silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of alkynol and 15 parts of hydrogen-containing silicone oil with the hydrogen content of 0.5 percent (wt%).
The preparation method is the same as example 1.
Comparative example 1
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000mPa.s, 30 parts of aluminum hydroxide, 13 parts of nano calcium carbonate and 1.5 parts of catalyst;
the component B comprises the following raw material components in parts by weight:
850 parts of hydroxyl silicone oil with the viscosity of 20000mPa.s, 15 parts of TDI terminated silicone oil, 30 parts of aluminum hydroxide, 3 parts of fumed silica, 1 part of alkynol and 9 parts of hydrogen-containing silicone oil;
other conditions were the same as in example 1.
Comparative example 2
A silicone foam material comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with viscosity of 20000 mPas, 25 parts of aluminum hydroxide, 20 parts of mica, 5 parts of nano calcium carbonate and 1.5 parts of platinum catalyst with platinum content of 5000 ppm;
the component B comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil with the viscosity of 20000mPa.s, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of alkynol and 9 parts of hydrogen-containing silicone oil with the hydrogen content of 0.8 percent (wt percent).
Other conditions were the same as in example 1.
The mechanical properties and the fire-retardant and flame-retardant properties of the silicone foams prepared in examples 1 to 5 and comparative examples 1 to 2 of the present invention were tested, and the test methods and test results were as follows:
test method
1. Mechanical properties
The test was carried out using an Instron model 5567 universal material testing machine manufactured by Instron corporation, USA, and the tensile strength was measured in accordance with GB/T528-2009.
2. Fire-proof performance
The mixture was ablated with a butane torch for 30 minutes, and the change of the ablated surface was observed.
3. Compressive strength
The test was carried out with reference to the method of GB/T88132008.
4. Density of foam
The measurement was carried out using a foam densitometer.
The test results are shown in table 1:
TABLE 1
Figure BDA0003286633820000091
Figure BDA0003286633820000101
According to the test results, the tensile strength of the prepared organic silicon fireproof plugging foam material is 0.33-0.66 Mpa, the density is low, the foam material has good mechanical properties and excellent fireproof and flame-retardant properties, and can be used for fireproof plugging of electric power construction equipment, foam blocking layers of new energy batteries, heat insulation layers of chemical equipment and the like. As can be seen from examples 1 to 5 and comparative example 1, the addition of the plate-like filler promotes the maintenance of the integrity of the shape of the ablation layer and the improvement of the fire-retardant property; as can be seen from examples 1 to 5 and comparative example 2, the isocyanate-terminated silicone oil is beneficial to improving the mechanical properties of the material, and meanwhile, the cost is not greatly increased.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (16)

1. An organosilicon foam material is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 1: 1-1: 2, wherein,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil, 10-40 parts of aluminum hydroxide, 2-20 parts of flaky filler, 5-10 parts of nano calcium carbonate and 1-3 parts of catalyst;
the component B comprises the following raw material components in parts by weight:
80-90 parts of hydroxyl silicone oil, 10-20 parts of isocyanate terminated silicone oil, 10-40 parts of aluminum hydroxide, 5-10 parts of fumed silica, 1-3 parts of inhibitor and 2-15 parts of hydrogen-containing silicone oil.
2. The silicone foam material of claim 1, comprising a component A and a component B, wherein the mass ratio of the component A to the component B is 1:1 to 1:2, wherein,
the component A comprises the following raw material components in parts by weight:
100 parts of hydroxyl silicone oil, 25 parts of aluminum hydroxide, 20 parts of flaky filler, 5 parts of nano calcium carbonate and 1.5 parts of catalyst;
the component B comprises the following raw material components in parts by weight:
85 parts of hydroxyl silicone oil, 15 parts of isocyanate-terminated silicone oil, 35 parts of aluminum hydroxide, 5 parts of fumed silica, 1 part of inhibitor and 9 parts of hydrogen-containing silicone oil.
3. The silicone foam of claim 1, wherein said plate-like filler is one or more of molybdenum dioxide, graphene, mica.
4. The silicone foam of claim 1, wherein the hydroxyl silicone oil has a viscosity of 500 to 20000 mpa.s.
5. The silicone foam of claim 1, wherein the catalyst is a platinum catalyst and the platinum content is 500 to 5000 ppm.
6. The silicone foam of claim 1, wherein said inhibitor is an alkynol or phenylacetylene.
7. The silicone foam of claim 1, wherein said isocyanate-terminated silicone oil is prepared by:
reacting diisocyanate and alpha, omega-dihydroxypropyl terminated silicone oil at room temperature under the catalysis of dibutyltin dilaurate, wherein the molar ratio of the diisocyanate to the alpha, omega-dihydroxypropyl terminated silicone oil is 1:1.
8. The silicone foam of claim 7, wherein dibutyltin dilaurate is added in an amount of 1% of the total mass of diisocyanate and α, ω -dihydroxypropyl terminated silicone oil.
9. The silicone foam of claim 7, wherein said diisocyanate is toluene diisocyanate TDI or hexamethylene diisocyanate HDI.
10. The silicone foam of claim 1, wherein said hydrogen-containing silicone oil has a hydrogen content of from 0.5% to 1.4%.
11. A process for the preparation of the silicone foam according to any one of claims 1 to 10, characterized in that it comprises the following steps:
stirring hydroxyl silicone oil, aluminum hydroxide, flaky filler and nano calcium carbonate to obtain a mixed solution 1;
grinding the mixed solution 1, adding a catalyst, and uniformly mixing to obtain a component A;
stirring hydroxyl silicone oil, isocyanate-terminated silicone oil, aluminum hydroxide, fumed silica, an inhibitor and hydrogen-containing silicone oil to obtain a mixed solution 2;
grinding the mixed solution 2 to obtain a component B;
and mixing and stirring the prepared component A and the component B uniformly to prepare the organic silicon foam material.
12. The method of claim 11, wherein the step of grinding the mixture 1 and the step of grinding the mixture 2 are performed at a grinding speed of 80 to 100r/min for 1 to 2 hours.
13. The method for preparing silicone foam material according to claim 11, wherein in the step of stirring hydroxyl silicone oil, aluminum hydroxide, flaky filler and nano calcium carbonate and the step of stirring hydroxyl silicone oil, isocyanate-terminated silicone oil, aluminum hydroxide, fumed silica, inhibitor and hydrogen-containing silicone oil, the stirring speed is 1000-1500 r/min, and the stirring time is 30-50 min.
14. Use of the silicone foam according to any one of claims 1 to 9 for fire blocking of electrical power construction equipment.
15. Use of the silicone foam of any one of claims 1 to 9 for a new energy battery foam barrier layer.
16. Use of the silicone foam according to any one of claims 1 to 9 for insulation of chemical equipment.
CN202111149944.1A 2021-09-29 2021-09-29 Organosilicon foam material, preparation method and application Pending CN113930076A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111149944.1A CN113930076A (en) 2021-09-29 2021-09-29 Organosilicon foam material, preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111149944.1A CN113930076A (en) 2021-09-29 2021-09-29 Organosilicon foam material, preparation method and application

Publications (1)

Publication Number Publication Date
CN113930076A true CN113930076A (en) 2022-01-14

Family

ID=79277432

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111149944.1A Pending CN113930076A (en) 2021-09-29 2021-09-29 Organosilicon foam material, preparation method and application

Country Status (1)

Country Link
CN (1) CN113930076A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115926742A (en) * 2022-12-02 2023-04-07 江苏中恒电子新材料有限公司 Organic silicon gel for waterproofing instruments and meters and preparation method thereof
WO2024000114A1 (en) * 2022-06-27 2024-01-04 Dow Silicones Corporation Organopolysiloxane foam with expanded perlite

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105504205A (en) * 2015-12-29 2016-04-20 浙江荣泰科技企业有限公司 Polysiloxane-polyurethane potting adhesive and preparation method thereof
CN105884267A (en) * 2016-04-12 2016-08-24 山东大学 Flame-retardant and drippage-free ceramization silicon rubber and preparation method thereof
WO2017070893A1 (en) * 2015-10-29 2017-05-04 国家纳米科学中心 Ceramic silicone rubber, preparation method and use thereof
CN106832274A (en) * 2015-12-05 2017-06-13 青岛纵横农业科技有限公司 A kind of preparation method with filling functional stuffing
CN109593464A (en) * 2018-11-09 2019-04-09 中国科学院化学研究所 A kind of organic silicon rubber coating of room curing and high temperature resistant, preparation method and application
CN111378285A (en) * 2020-04-30 2020-07-07 新纳奇材料科技江苏有限公司 High-strength high-flame-retardant organic silicon foam material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017070893A1 (en) * 2015-10-29 2017-05-04 国家纳米科学中心 Ceramic silicone rubber, preparation method and use thereof
CN106832274A (en) * 2015-12-05 2017-06-13 青岛纵横农业科技有限公司 A kind of preparation method with filling functional stuffing
CN105504205A (en) * 2015-12-29 2016-04-20 浙江荣泰科技企业有限公司 Polysiloxane-polyurethane potting adhesive and preparation method thereof
CN105884267A (en) * 2016-04-12 2016-08-24 山东大学 Flame-retardant and drippage-free ceramization silicon rubber and preparation method thereof
CN109593464A (en) * 2018-11-09 2019-04-09 中国科学院化学研究所 A kind of organic silicon rubber coating of room curing and high temperature resistant, preparation method and application
CN111378285A (en) * 2020-04-30 2020-07-07 新纳奇材料科技江苏有限公司 High-strength high-flame-retardant organic silicon foam material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
朱丹: "新型有机硅橡胶的制备与性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *
王志明: "《化工常识》", 30 September 1975 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024000114A1 (en) * 2022-06-27 2024-01-04 Dow Silicones Corporation Organopolysiloxane foam with expanded perlite
CN115926742A (en) * 2022-12-02 2023-04-07 江苏中恒电子新材料有限公司 Organic silicon gel for waterproofing instruments and meters and preparation method thereof

Similar Documents

Publication Publication Date Title
CN113930076A (en) Organosilicon foam material, preparation method and application
CN105860537B (en) High-flame-retardant organic silicon sponge material and preparation method thereof
CN111378285B (en) High-strength high-flame-retardant organic silicon foam material and preparation method thereof
CN109575605A (en) A kind of flame retardant silica gel foam and preparation method thereof
CN101307129B (en) Polyurethane/organic montmorillonite nano composite material and method for preparing same
CN117844255A (en) Silica gel sheet and preparation method and application thereof
CN108276774A (en) A kind of organosilicon composition, foam and the porous, expanded material of organosilicon prepared by the composition, foam
CN110684358A (en) Filling foaming encapsulation silica gel for new energy power battery, preparation method and application
Song et al. Preparation and characterization of epoxy resin modified with alkoxysilane‐functionalized poly (urethane‐imide) by the sol–gel process
CN112795198B (en) High-flame-retardant organic silicon foam sheet and preparation method thereof
CN110894363A (en) Tear-resistant organic silicon foam material and preparation method thereof
CN105778511A (en) Room-temperature vulcanized organic silicon foam sealant and preparation method thereof
CN117683357A (en) High-resilience flame-retardant silicone rubber foam and preparation method thereof
CN112940335A (en) Preparation method of porous silicon rubber material
CN111138864A (en) Fluorine-containing oil-resistant anti-swelling silicone rubber foam material and preparation method thereof
CN110452661B (en) Self-defoaming and dehydrogenation type oil-resistant high-temperature-resistant fluorine-silicon sealant and preparation method thereof
CN113122001A (en) Fireproof and heat-insulating organic silicon foam used between battery cores and preparation method thereof
CN116178961B (en) Closed-cell type flame-retardant heat-conducting foam silica gel sheet and preparation method thereof
CN111574673A (en) Environment-friendly heat-conducting polyurethane foam, preparation method thereof and adhesive tape
CN116355276B (en) Halogen-free silica gel material with core-shell structure, preparation method and application
CN112940671B (en) Preparation method of organosilicon foam material with high flame retardant property
CN117430780B (en) Flame retardant rigid polyurethane foam and preparation method thereof
CN112625206B (en) Polyurethane expansion type fireproof plugging sheet, preparation method thereof and sealing system
CN112940672B (en) Preparation method of organosilicon foam material with high foaming performance
KR102594257B1 (en) Manufacturing method of porous polyurethane foam having excellent flame retardancy

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20220114