CN113930076A - Organosilicon foam material, preparation method and application - Google Patents
Organosilicon foam material, preparation method and application Download PDFInfo
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- 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
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- 239000006261 foam material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920002545 silicone oil Polymers 0.000 claims abstract description 93
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 40
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 39
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 239000012948 isocyanate Substances 0.000 claims abstract description 4
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 32
- 229920002323 Silicone foam Polymers 0.000 claims description 31
- 239000013514 silicone foam Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 17
- 229910052697 platinum Inorganic materials 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 15
- 239000006260 foam Substances 0.000 claims description 10
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 8
- 125000005442 diisocyanate group Chemical group 0.000 claims description 8
- 230000000903 blocking effect Effects 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000010445 mica Substances 0.000 claims description 7
- 229910052618 mica group Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 claims description 4
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical group CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- -1 Si-H Chemical group 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 239000003063 flame retardant Substances 0.000 description 8
- 238000002679 ablation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229920002379 silicone rubber Polymers 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
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- 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
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- 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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- 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
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- 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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- 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
- C08J2483/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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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
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
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.
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