CN113897153A - Flame retardant, organic silicon pouring sealant, and preparation method and application thereof - Google Patents
Flame retardant, organic silicon pouring sealant, and preparation method and application thereof Download PDFInfo
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- CN113897153A CN113897153A CN202111205580.4A CN202111205580A CN113897153A CN 113897153 A CN113897153 A CN 113897153A CN 202111205580 A CN202111205580 A CN 202111205580A CN 113897153 A CN113897153 A CN 113897153A
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- component
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- pouring sealant
- silicone oil
- organic silicon
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Links
- 239000000565 sealant Substances 0.000 title claims abstract description 55
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 46
- 239000010703 silicon Substances 0.000 title claims abstract description 46
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- 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 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims description 64
- 229920002554 vinyl polymer Polymers 0.000 claims description 57
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000001257 hydrogen Substances 0.000 claims description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 20
- 230000002209 hydrophobic effect Effects 0.000 claims description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000006229 carbon black Substances 0.000 claims description 14
- 238000004382 potting Methods 0.000 claims description 14
- 239000000853 adhesive Substances 0.000 claims description 13
- 230000001070 adhesive effect Effects 0.000 claims description 13
- 229920001296 polysiloxane Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- 239000004970 Chain extender Substances 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 239000003112 inhibitor Substances 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- -1 polysiloxane Polymers 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 2
- 150000002688 maleic acid derivatives Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract description 16
- 229920000877 Melamine resin Polymers 0.000 abstract description 15
- 229920002379 silicone rubber Polymers 0.000 abstract description 8
- 150000007974 melamines Chemical class 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 238000004062 sedimentation Methods 0.000 abstract description 6
- 239000004677 Nylon Substances 0.000 abstract description 5
- 239000007977 PBT buffer Substances 0.000 abstract description 5
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- 229920001778 nylon Polymers 0.000 abstract description 5
- 239000012994 photoredox catalyst Substances 0.000 abstract description 5
- 239000004417 polycarbonate Substances 0.000 abstract description 5
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 5
- 239000010935 stainless steel Substances 0.000 abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 5
- 238000002485 combustion reaction Methods 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000203 mixture Substances 0.000 description 11
- DBAMUTGXJAWDEA-UHFFFAOYSA-N Butynol Chemical compound CCC#CO DBAMUTGXJAWDEA-UHFFFAOYSA-N 0.000 description 9
- 230000006872 improvement Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002318 adhesion promoter Substances 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 description 1
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 description 1
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- QMCVOSQFZZCSLN-QXMHVHEDSA-N dihexyl (z)-but-2-enedioate Chemical compound CCCCCCOC(=O)\C=C/C(=O)OCCCCCC QMCVOSQFZZCSLN-QXMHVHEDSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Abstract
The invention belongs to the technical field of high polymer materials, and discloses an organic silicon pouring sealant and a preparation method and application thereof, wherein raw material components for preparing the organic silicon pouring sealant comprise a component A and a component B; the raw material components for preparing the component A comprise a flame retardant, and the structure of the flame retardant is shown as the formula (1):
wherein R is1、R2Each independently selected from the group of structures:
or
R3Is a group selected from the following structures:
or
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an organic silicon pouring sealant as well as a preparation method and application thereof.
Background
With the development of the electronic and electrical industry, electronic components, devices, instruments and meters are widely used in the electronic industry. Because the working environment of many electronic devices is complex and variable, sometimes even extremely severe natural conditions are encountered, in order to protect electronic components and integrated circuits from the working environment and to improve the electrical performance and stability of electronic devices, the electronic devices often need to be encapsulated and protected. The encapsulation can strengthen the integrity of electronic components, prevent the erosion of moisture, dust, harmful gas and the like to the integrated circuit, improve the insulating property between the internal elements of the electronic equipment and the circuit, reduce the influence of external vibration and impact on the electronic devices, stabilize the parameters of the electronic components, and be favorable for the miniaturization and the light weight of the electronic devices.
The addition type organic silicon potting adhesive has the advantages of less catalyst consumption during curing, no byproduct generation, deep curing, high dimensional stability of a cured product, low linear shrinkage rate and excellent chemical stability, and becomes one of high-performance potting materials. Although the addition type organic silicon pouring sealant has incomparable advantages with other pouring materials, the common organic silicon pouring sealant has the defects of poor flame retardant property, poor adhesion to base materials and the like, and the application of the addition type organic silicon pouring sealant is seriously influenced.
Generally, flame-retardant fillers, flame retardants and silane coupling agents are added into addition type silicone rubber to improve the flame retardance and the adhesion of the organic silicon pouring sealant, but due to the fact that the added flame-retardant fillers are high in density and poor in compatibility with the silicone rubber, the organic silicon pouring sealant can be seriously settled in the transportation and storage process, the powder-liquid separation condition seriously affects the use and product performance, and the market demand cannot be met.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides the flame retardant, the organic silicon pouring sealant, the preparation method and the application thereof, the obtained organic silicon pouring sealant can be stored without sedimentation phenomenon, the vertical combustion reaches UL-94V-0 level, and the organic silicon pouring sealant has good adhesion to base materials such as aluminum materials, stainless steel, PET, PC, PBT, ABS, nylon and the like.
The invention has the following inventive concept: according to the invention, the component A and the component B are compounded to prepare the raw material component of the component A, wherein the flame retardant has a structural formula shown in formula (1), and the melamine is modified by using the silane coupling agent, so that the compatibility of the melamine and silicon rubber can be effectively improved, and the anti-settling performance of the modified melamine in an organic silicon pouring sealant product can be improved; meanwhile, epoxy and high-activity siloxy are introduced, so that the organosilicon potting adhesive can react with active groups on the surface of a base material on the premise of ensuring that the organosilicon potting adhesive product has higher flame retardant property, and the organosilicon potting adhesive has good adhesion. The obtained organic silicon pouring sealant can be stored without sedimentation, vertical combustion reaches UL-94V-0 level, and the organic silicon pouring sealant has good adhesion to aluminum materials, stainless steel, PET, PC, PBT, ABS, nylon and other base materials.
In a first aspect of the invention, a flame retardant is provided.
Specifically, the structure of the flame retardant is shown as the formula (1):
wherein R is1、R2Each independently selected from the group of structures:
R3is a group selected from the following structures:
the reaction process is concretely as follows:
and
mixing with ethanol solution of quaternary ammonium salt at about 78 deg.C, removing low content, and filtering to obtain product of formula (1) (wherein R is1And R2Are all made of
R3Is composed of
)。
Furthermore, the flame retardant is modified melamine with a structure shown in a formula (1), and therefore, the melamine is a nitrogen flame retardant which has lower density and excellent flame retardant property compared with flame retardant fillers such as aluminum hydroxide and the like, but the melamine is easy to settle in the transportation and storage processes due to poor compatibility of the melamine and silicon rubber.
Therefore, the invention can effectively improve the compatibility of the melamine and the silicon rubber and improve the anti-settling performance in the organic silicon pouring sealant product by modifying the melamine by using the silane coupling agent; meanwhile, epoxy and high-activity siloxy are introduced, so that the organosilicon potting adhesive can react with active groups on the surface of a base material on the premise of ensuring that the organosilicon potting adhesive product has higher flame retardant property, and the organosilicon potting adhesive has good adhesion, wherein the active groups refer to groups which are easy to chemically react or form hydrogen bonds on the surface of the base material such as hydroxyl, ester, carbonyl, amide and the like.
The second aspect of the present invention is to provide an organosilicon potting adhesive.
Specifically, the raw material components for preparing the organic silicon pouring sealant comprise a component A and a component B; the raw material component for preparing the component A comprises the flame retardant disclosed by the invention. Specifically, the weight parts ratio of the A component to the B component is about 1: 1; the modified melamine is used as a flame retardant, so that the compatibility of the melamine and the silicon rubber can be effectively improved, and the anti-settling performance of the modified melamine in an organic silicon pouring sealant product can be improved.
As a further improvement of the above scheme, the component a further comprises vinyl silicone oil and a platinum catalyst; preferably, the raw material components for preparing the A component further comprise 50 parts by weight of vinyl silicone oil, 10-50 parts by weight of flame retardant and 0.2-2 parts by weight of platinum catalyst.
As a further improvement of the above aspect, the platinum catalyst is selected from at least one of an isopropyl alcohol solution of chloroplatinic acid, a platinum-vinyl complex, or a platinum-alkynyl complex.
As a further improvement of the scheme, the component B comprises vinyl silicone oil, hydrophobic white carbon black, a cross-linking agent, a chain extender, an inhibitor and a tackifier; preferably, the raw material components for preparing the component B comprise 50 parts by weight of vinyl silicone oil, 3-15 parts by weight of hydrophobic white carbon black, 3-15 parts by weight of cross-linking agent, 3-15 parts by weight of chain extender, 0.1-2 parts by weight of inhibitor and 0.1-10 parts by weight of tackifier.
As a further improvement of the scheme, the structure of the tackifier is shown as a formula (2):
wherein M is1Is composed of
M2(ii) select-CH2CH2COOCH3、-CH2CH2COOCH2CH3、-CH2CH2COOCH2CH2CH3or-CH2CH2COOCH2CH2CH2CH3The compound is prepared from tetramethylcyclotetrasiloxane, allyl glycidyl ether and acrylate through conventional hydrosilylation reaction.
Specifically, the adhesion promoter is used for synergistically modifying the melamine, and the modified melamine contains a large amount of alkoxy groups and ester groups contained in the adhesion promoter, so that the adhesion performance to a base material is further effectively improved.
As a further improvement of the scheme, the vinyl silicone oil has a vinyl content of 0.2-2 wt% and a viscosity of 50-6000 mPa. Specifically, vinyl silicone oil with lower viscosity is selected to be matched with vinyl silicone oil with high and low viscosity for use, so that the organosilicon pouring sealant has low viscosity and proper strength.
As a further improvement of the above scheme, the hydrophobic silica is obtained by treating the hydrophobic silica with a hydrophobic silica treating agent, wherein the hydrophobic silica treating agent is at least one selected from hexamethyldisilazane, tetramethyldivinylsilazane, hexamethyldisiloxane or vinyltrimethoxysilane.
Further, the cross-linking agent comprises hydrogen-containing silicone oil; preferably, the hydrogen-containing silicone oil contains 0.2-0.7% of hydrogen by mass and has a viscosity of 18-200 mPa · s.
Further, the chain extender comprises hydrogen-terminated silicone oil with the viscosity of 2-10 mPa.
Further, the inhibitor is selected from at least one of polyvinyl polysiloxane, alkynol compounds or maleate compounds. Specifically, the polyvinyl polysiloxane comprises tetravinyl tetramethylcyclotetrasiloxane; the alkynol compound comprises butynol and/or ethyncyclohexanol; the maleate ester compound comprises dihexyl maleate and the like.
The third aspect of the invention provides a preparation method of the organic silicon pouring sealant, which comprises the following steps:
preparing a component A: taking vinyl silicone oil and a flame retardant according to a formula, stirring and mixing, adding a platinum catalyst and a tackifier, stirring in vacuum, and filtering to remove impurities to obtain a component A;
preparing a component B: mixing vinyl silicone oil and hydrophobic white carbon black according to a formula, adding a cross-linking agent, a chain extender and an inhibitor, stirring in vacuum, and filtering impurities to obtain a component B;
and mixing the component A and the component B to prepare the organic silicon pouring sealant.
Further preferably, the parts by weight ratio of said a component to said B component is about 1: 1. specifically, a planetary stirrer or a high-speed dispersion machine is adopted in the stirring process; the vacuum stirring time is 0.5-2 h.
The fourth aspect of the invention provides an application of the organic silicon pouring sealant.
Preferably, the organic silicon pouring sealant disclosed by the invention is applied to the electronic industry.
Further preferably, the electronics industry includes electronic components, electronic devices, electronic instruments, electronic meters, and the like.
Compared with the prior art, the invention has the following beneficial effects:
1) according to the invention, the component A and the component B are compounded, wherein the flame retardant in the raw material component for preparing the component A adopts the modified melamine with the structure shown in the formula (1), so that the compatibility of the melamine and silicon rubber can be effectively improved, and the anti-settling property in an organic silicon pouring sealant product can be improved;
2) the invention introduces epoxy and high-activity siloxy, and can react with active groups on the surface of a base material on the premise of ensuring that an organosilicon pouring sealant product has higher flame retardant property, so that the organosilicon pouring sealant has good adhesion.
3) The organic silicon pouring sealant obtained by the invention has no sedimentation phenomenon in the storage process, achieves UL-94V-0 level in vertical combustion, has good adhesion to base materials such as aluminum materials, stainless steel, PET, PC, PBT, ABS, nylon and the like, has wide application prospect, and meets the market demand.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
An organic silicon pouring sealant, which is prepared from raw material components comprising a component A and a component B; the component A comprises 50 parts of vinyl silicone oil with the viscosity of 1000 mPas (500 mPas and 2000 mPas are mixed according to the ratio of 1: 1), and 20 parts of flame retardant (R1、R2Are all made of
R3Is composed of
) And 1 part of a platinum-vinyl complex; the component B comprises 50 parts of vinyl silicone oil with the viscosity of 1000 mPas (500 mPas and 2000 mPas are mixed according to the ratio of 1: 1), 15 parts of hydrophobic white carbon black treated by hexamethyldisilazane, 6 parts of hydrogen-containing silicone oil with the hydrogen mass fraction of 0.36 percent and the viscosity of 40 mPas, and 3 parts of tackifier (M)1Is composed of
M2is-CH2CH2COOCH3) 10 parts of hydrogen-terminated silicone oil with the viscosity of 5mPa & s, and 0.2 part of butynol; the weight ratio of the component A to the component B is 1: 1.
a preparation method of an organic silicon pouring sealant comprises the following steps:
preparing a component A: 50 parts of a vinyl silicone oil mixture having a viscosity of 1000 mPas (500 mPas and 2000 mPas vinyl silicone oil 1:1 mixed), 20 parts of a flame retardant (R1、R2Are all made of
R3Is composed of
) Adding into a planetary mixer or a high-speed dispersion machine, mixing uniformly, adding 1 part of platinum-vinyl complex and 3 parts of tackifier (M)1Is composed of
M2is-CH2CH2COOCH3) Stirring for 1h in vacuum, and filtering impurities to obtain a component A;
preparing a component B: 50 parts of vinyl silicone oil mixture with the viscosity of 1000 mPas (500 mPas and 2000 mPas vinyl silicone oil are mixed in a ratio of 1: 1), 15 parts of hydrophobic white carbon black treated by hexamethyldisilazane are uniformly mixed, 6 parts of hydrogen-containing silicone oil with the hydrogen mass fraction of 0.36% and the viscosity of 40 mPas, 10 parts of hydrogen-terminated silicone oil with the viscosity of 5 mPas and 0.2 part of butynol are added and uniformly mixed, the mixture is stirred in vacuum for 1 hour, and a component B is obtained after impurities are filtered;
respectively obtaining a component A and a component B, wherein the component A and the component B are 1:1 to obtain the finished product 1 of the organic silicon pouring sealant in the embodiment.
Example 2
An organic silicon pouring sealant, which is prepared from raw material components comprising a component A and a component B; the component A comprises 50 parts of vinyl silicone oil with the viscosity of 1000 mPas (500 mPas and 2000 mPas are mixed according to the ratio of 1: 1), and 50 parts of flame retardant (R1、R2Are all made of
R3Is composed of
) And 1 part of a platinum-vinyl complex; the component B comprises 50 parts of vinyl silicone oil with the viscosity of 1000 mPas (500 mPas and 2000 mPas are mixed according to the ratio of 1: 1), 5 parts of hydrophobic white carbon black treated by hexamethyldisilazane, 6 parts of hydrogen-containing silicone oil with the hydrogen mass fraction of 0.36 percent and the viscosity of 40 mPas, and 4 parts of tackifier (M)1Is composed of
M2is-CH2CH2COOCH2CH3) 10 parts of hydrogen-terminated silicone oil with the viscosity of 5mPa & s, and 0.2 part of butynol; the weight ratio of the component A to the component B is 1: 1.
a preparation method of an organic silicon pouring sealant comprises the following steps:
preparing a component A: 50 parts of a vinyl silicone oil mixture having a viscosity of 1000 mPas (500 mPas and 2000 mPas vinyl silicone oil 1: 1) and 50 parts of a flame retardant (R1、R2Are all made of
R3Is composed of
) Adding the mixture into a planetary stirrer or a high-speed dispersion machine, uniformly mixing, adding 1 part of platinum-vinyl complex, stirring for 1 hour in vacuum, and filtering impurities to obtain a component A;
preparing a component B: 50 parts of a vinyl silicone oil mixture having a viscosity of 1000 mPas (500 mPas and 2000 mPas vinyl silicone oil 1: 1) and 5 parts of hydrophobic white carbon black treated with hexamethyldisilazane were mixed uniformly, and 6 parts of a hydrogen-containing silicone oil having a hydrogen content of 0.36% by mass and a viscosity of 40 mPas and 4 parts of a thickener (M)1Is composed of
M2is-CH2CH2COOCH2CH3) 10 parts of hydrogen-terminated silicone oil with the viscosity of 5mPa & s and 0.2 part of butynol are uniformly mixed, stirred for 1 hour in vacuum, and then filtered to obtain a component B;
respectively obtaining a component A and a component B, wherein the component A and the component B are 1:1 to obtain the finished product 2 of the organic silicon pouring sealant in the embodiment.
Example 3
An organic silicon pouring sealant, which is prepared from raw material components comprising a component A and a component B; the component A comprises 50 parts of vinyl silicone oil with the viscosity of 3000 mPas (300 mPas and 6000 mPas are mixed according to the ratio of 1: 3), and 20 parts of flame retardant (R1、R2Are all made of
R3Is composed of
) And 1 part of a platinum-vinyl complex; the component B comprises 50 parts of vinyl silicone oil with the viscosity of 3000 mPas (300 mPas is mixed with vinyl silicone oil with the viscosity of 6000 mPas according to the ratio of 1: 3), 5 parts of hydrophobic white carbon black treated by hexamethyldisilazane, 12 parts of hydrogen-containing silicone oil with the hydrogen mass fraction of 0.18 percent and the viscosity of 80 mPas, and 6 parts of tackifier (M)1Is composed of
M2is-CH2CH2COOCH2CH2CH3) 5 parts of hydrogen-terminated silicone oil with the viscosity of 7mPa & s, and 0.2 part of butynol; the weight ratio of the component A to the component B is 1: 1.
a preparation method of an organic silicon pouring sealant comprises the following steps:
preparing a component A: 50 parts of a vinyl silicone oil mixture having a viscosity of 3000 mPas (300 mPas and 6000 mPas vinyl silicone oil 1: 3), 20 parts of a flame retardant (R)1、R2Are all made of
R3Is composed of
) Adding the mixture into a planetary stirrer or a high-speed dispersion machine, uniformly mixing, adding 1 part of platinum-vinyl complex, stirring for 1 hour in vacuum, and filtering impurities to obtain a component A;
preparing a component B: 50 parts of a vinyl silicone oil mixture having a viscosity of 3000 mPas (300 mPas and 6000 mPas vinyl silicone oil 1: 3) and 5 parts of hydrophobic white carbon black treated with hexamethyldisilazane were mixed uniformly, and 12 parts of a hydrogen-containing silicone oil having a hydrogen content of 0.18% by mass and a viscosity of 80 mPas and 6 parts of a thickener (M)1Is composed of
M2is-CH2CH2COOCH2CH2CH3) 5 parts of hydrogen-terminated silicone oil with the viscosity of 7 mPas and 0.2 part of butynol are uniformly mixed and vacuumizedStirring for 1 hour, and filtering to remove impurities to obtain a component B;
respectively obtaining a component A and a component B, wherein the component A and the component B are 1:1 to obtain the finished product 3 of the organic silicon pouring sealant in the embodiment.
Example 4
An organic silicon pouring sealant, which is prepared from raw material components comprising a component A and a component B; the component A comprises 50 parts of vinyl silicone oil with the viscosity of 3000 mPas (300 mPas and 6000 mPas are mixed according to the ratio of 1: 3), and 20 parts of flame retardant (R1、R2Are all made of
R3Is composed of
) And 1 part of a platinum-vinyl complex; the component B comprises 50 parts of vinyl silicone oil with the viscosity of 3000 mPas (300 mPas is mixed with vinyl silicone oil with the viscosity of 6000 mPas according to the ratio of 1: 3), 5 parts of hydrophobic white carbon black treated by hexamethyldisilazane, 4 parts of hydrogen-containing silicone oil with the hydrogen mass fraction of 0.6% and the viscosity of 80 mPas, and 8 parts of tackifier (M)1Is composed of
M2is-CH2CH2COOCH2CH2CH2CH3) 12 parts of hydrogen-terminated silicone oil with the viscosity of 7mPa & s, and 0.2 part of butynol; the weight ratio of the component A to the component B is 1: 1.
a preparation method of an organic silicon pouring sealant comprises the following steps:
preparing a component A: 50 parts of a vinyl silicone oil mixture having a viscosity of 3000 mPas (300 mPas and 6000 mPas vinyl silicone oil 1: 3), 20 parts of a flame retardant (R)1、R2Are all made of
R3Is composed of
) AddingMixing in a planetary mixer or a high-speed disperser, adding 1 part of platinum-vinyl complex, stirring in vacuum for 1h, and filtering to remove impurities to obtain component A;
preparing a component B: 50 parts of a vinyl silicone oil mixture having a viscosity of 3000 mPas (300 mPas and 6000 mPas vinyl silicone oil 1: 3) and 5 parts of hydrophobic white carbon black treated with hexamethyldisilazane were mixed uniformly, and 4 parts of a hydrogen-containing silicone oil having a hydrogen content of 0.6 mass% and a viscosity of 80 mPas and 8 parts of a thickener (M)1Is composed of
M2is-CH2CH2COOCH2CH2CH2CH3) 12 parts of hydrogen-terminated silicone oil with the viscosity of 7mPa & s and 0.2 part of butynol are uniformly mixed, stirred for 1 hour in vacuum, and then filtered to obtain a component B;
respectively obtaining a component A and a component B, wherein the component A and the component B are 1:1 to obtain the finished product 4 of the organic silicon pouring sealant in the embodiment.
Example 5 (without tackifier)
The difference between example 5 and example 4 is that no tackifier is added in example 5, and other preparation raw materials and preparation processes are the same, so that example finished product 5 of the organosilicon potting adhesive is prepared.
Comparative example 1 (using aluminum hydroxide as flame retardant)
The difference between the comparative example 1 and the example 4 is that the finished product 1 of the organosilicon potting adhesive is prepared by adopting aluminum hydroxide as a flame retardant in the comparative example 1 and adopting the same other preparation raw materials and preparation processes.
Comparative example 2 (using melamine as flame retardant)
The difference between the comparative example 2 and the example 4 is that the finished product 2 of the comparative example of the organic silicon pouring sealant is prepared by adopting melamine as a flame retardant in the comparative example 2 and adopting the same other preparation raw materials and preparation processes.
Comparative example 3 (melamine as flame retardant, without tackifier)
The difference between the comparative example 3 and the example 4 is that in the comparative example 3, melamine is used as a flame retardant, no tackifier is added, and other preparation raw materials and preparation processes are the same, so that a finished product 3 of the comparative example of the organic silicon pouring sealant is prepared.
Product Performance and Effect testing
The silicone potting adhesive finished products obtained in examples 1 to 5 and comparative examples 1 to 3 were tested for sedimentation (9 months of storage at room temperature), flame retardant rating, adhesion, and the like. The results obtained are shown in table 1 below.
TABLE 1
As can be seen from Table 1, the silicone pouring sealant prepared in examples 1-5 can be stored without sedimentation, vertical burning reaches UL-94V-0 level, and has good adhesion to aluminum materials, stainless steel, PET, PC, PBT, ABS, nylon and other substrates, and the pouring sealant prepared in examples 1-5 has better comprehensive properties than those prepared in comparative examples 1-3.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (10)
1. A flame retardant is characterized in that the structure is shown as formula (1):
wherein R is1、R2Each independently selected from the group of structures:
R3is a group selected from the following structures:
2. the organic silicon pouring sealant is characterized in that raw material components for preparing the organic silicon pouring sealant comprise a component A and a component B; the raw material components for preparing the A component comprise the flame retardant of claim 1.
3. The silicone pouring sealant according to claim 2, wherein the component a further comprises vinyl silicone oil and a platinum catalyst; preferably, the raw material components for preparing the A component further comprise 50 parts by weight of vinyl silicone oil, 10-50 parts by weight of flame retardant and 0.2-2 parts by weight of platinum catalyst.
4. The silicone potting adhesive of claim 3, wherein the platinum catalyst is selected from at least one of an isopropanol solution of chloroplatinic acid, a platinum-vinyl complex, or a platinum-alkynyl complex.
5. The organic silicon pouring sealant as claimed in claim 2, wherein the component B comprises vinyl silicone oil, hydrophobic white carbon black, a cross-linking agent, a chain extender, an inhibitor and a tackifier; preferably, the raw material components for preparing the component B comprise 50 parts by weight of vinyl silicone oil, 3-15 parts by weight of hydrophobic white carbon black, 3-15 parts by weight of cross-linking agent, 3-15 parts by weight of chain extender, 0.1-2 parts by weight of inhibitor and 0.1-10 parts by weight of tackifier.
6. The silicone pouring sealant as claimed in claim 5, wherein the structure of the tackifier is as shown in formula (2):
wherein M is1Is composed of
M2(ii) select-CH2CH2COOCH3、-CH2CH2COOCH2CH3、-CH2CH2COOCH2CH2CH3or-CH2CH2COOCH2CH2CH2CH3。
7. The silicone pouring sealant according to claim 3 or 5, wherein the vinyl silicone oil has a vinyl content of 0.2 wt% to 2 wt% and a viscosity of 50 to 6000mPa · s.
8. The silicone pouring sealant according to claim 5, wherein the hydrophobic silica is obtained by treating hydrophobic silica with a treating agent, and the treating agent is at least one of hexamethyldisilazane, tetramethyldivinylsilazane, hexamethyldisiloxane, or vinyltrimethoxysilane; the cross-linking agent comprises hydrogen-containing silicone oil; the hydrogen-containing silicone oil contains 0.2-0.7% of hydrogen by mass and has a viscosity of 18-200 mPa & s; the chain extender comprises hydrogen-terminated silicone oil with the viscosity of 2-10mPa & s; the inhibitor is at least one of polyvinyl polysiloxane, alkynol compounds or maleate compounds.
9. The method for preparing the silicone pouring sealant as claimed in any of claims 2 to 8, characterized by comprising the following steps:
preparing a component A: taking vinyl silicone oil and a flame retardant according to a formula, stirring and mixing, adding a platinum catalyst and a tackifier, stirring in vacuum, and filtering to remove impurities to obtain a component A;
preparing a component B: mixing vinyl silicone oil and hydrophobic white carbon black according to a formula, adding a cross-linking agent, a chain extender and an inhibitor, stirring in vacuum, and filtering impurities to obtain a component B;
and mixing the component A and the component B to prepare the organic silicon pouring sealant.
10. Use of the silicone potting adhesive of any of claims 2 to 8 in an electronic device.
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