CN110452661A - A kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant and preparation method thereof - Google Patents

A kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant and preparation method thereof Download PDF

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CN110452661A
CN110452661A CN201910787392.3A CN201910787392A CN110452661A CN 110452661 A CN110452661 A CN 110452661A CN 201910787392 A CN201910787392 A CN 201910787392A CN 110452661 A CN110452661 A CN 110452661A
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defoaming
self
silicone encapsulant
resistant high
type oil
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CN110452661B (en
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高元峰
吴松华
秦蓬波
章谏正
鲍传磊
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AECC Beijing Institute of Aeronautical Materials
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    • 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
    • C09J183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2265—Oxides; Hydroxides of metals of iron
    • C08K2003/2272—Ferric oxide (Fe2O3)
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/016—Additives defined by their aspect ratio
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2003/1034—Materials or components characterised by specific properties
    • C09K2003/1078—Fire-resistant, heat-resistant materials

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention belongs to high molecular material and its production technical field, it is related to a kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant and preparation method thereof.It is mixed by two components of base cream and vulcanizing agent, the component proportion of base cream and vulcanizing agent are as follows: base cream 99%, vulcanizing agent 1%: the liquid fluorosilicone rubber of the base cream is using hydroxy-end capped trifluompropyl methyl polysiloxane, and viscosity is between 20Pa.s-82Pa.s；The titanium dioxide filler is needle-shaped, draw ratio is 10:1 to 25:1, using self-defoaming formula technique, so that homogeneous after sealant vulcanization, performance is stablized, it uses liquid trifluompropyl methyl polysiloxane and prepares dehydrogenation type sealant for liquid raw rubber, there is good heatproof oil resistance.

Description

A kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant and preparation method thereof
Technical field
The invention belongs to high molecular material and its production technical fields, are related to a kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine Silicone encapsulant and preparation method thereof.The sealant has good self-defoaming performance, sulphur can be discharged while room temperature vulcanization The hydrogen generated during changing can be used for fuel tanker sealing and electric appliance encapsulating.
Background technique
With being constantly progressive for the development of aircraft industry, especially the 5th generation fighter plane and unmanned air vehicle technique, to aviation fluorine The performance requirement of silicone encapsulant is also higher and higher, especially the examination of the high temperature resistance to fluorine silicone encapsulant and oil resistance. From the point of view of current research achievement both domestic and external and product, there is dehydrogenation type fluorine silicone encapsulant best high temperature resistance (to make for a long time With 230 DEG C of temperature, 300 DEG C of short-period used temperature) and resistance to closed thermal degradation performance.
However, being directed to the fluorine silicone encapsulant of the encapsulating of fuel tanker position or electronic equipment at present, fuel oil steaming can only be resistant to Vapour is not resistant to the direct immersion of fuel oil, limits its further application.The reason is that: existing dehydrogenation type fluorine silicon The liquid fluorosilicone rubber that sealant uses is trifluoro propyl methylsiloxane-dimethyl siloxane copolymer (degree of polymerization ratio For 1:1), fluorine-containing mass fraction is only 16% (mass fraction)；According to trifluompropyl methyl polysiloxane as liquid fluorine silicon Rubber, fluorine content can be promoted to 32%, have an extraordinary oil resistance, but be difficult to due to the hydrogen in sulfidation and When be discharged, lead to the decline of service performance.Therefore, the row's bubble technology for developing the dehydrogenation type room temperature vulcanization sealant of high fluorinated volume is The key points and difficulties in the field at present.
The report about fluorine silicone encapsulant: room temperature sulphur is disclosed on " organosilicon material " 2011, Vol.25, No.2:76-79 Change the research of the resistance to jet fuel performance of fluorine silicone encapsulant.The paper is described in detail the molecular weight of fluorine silicon liquid body rubber, fluorinated volume, Influence of the vulcanizing system to the heat-resisting oil resistance of fluorine silicone encapsulant.Author thinks: oil resistant characteristic is influenced close by base rubber fluorinated volume It cuts, dehydrogenation type vulcanizing system heat resistance is best.
The report about fluorine silicone encapsulant foam performance is disclosed on " bonding " 2013, Vol.5, No.5:055-058: raw Influence of the glue side group structure to RTV organosilicon foaming sealant performance.The different side group silica gel of the research play-by-play are in dehydrogenation Foam performance when vulcanization, author think different side groups to the density of foam seal agent, foaming coefficient, Porosity Rate Influence basic one It causes, is not influenced by side group.
Preparation and the correlated performance of the sealant of different fluorinated volumes are reported in the research of above-mentioned dehydrogenation type sealing material. In existing research, do not sealed about the self-defoaming that trifluompropyl methyl polysiloxane is prepared as liquid fluorosilicone rubber The report of agent.
Chinese invention patent CN105441020 discloses a kind of aircraft integral tank sealant, and the sealant is with vinyl The trifluompropyl methyl polysiloxane of end group cooperates inorganic filler as base rubber, and the auxiliary agents such as heat-resistant agent can be grown at 250 DEG C Phase uses.
Chinese invention patent CN105086743 discloses a kind of fluorine silicone encapsulant of solvent of resistance to fuel oil, and the sealant is with hydroxyl The trifluompropyl methyl polysiloxane of base sealing end is as base rubber, using white carbon black and nanometer calcium carbonate as inorganic filler, using de- Alcohol type vulcanizing system, only 10% volume change after fuel oil immersion
The fluorine fluosilicic silicone encapsulant that above-mentioned patent is related to relates generally to the research in vulcanizing system and performance formula, about disappearing The research of bubble function does not have mentioned.Due to using add-on type and depickling type vulcanizing system, processing performance and resistance to is used Warm nature can be limited by use condition, not be able to satisfy the harsh working condition of aircraft utilization and maintenance.
Summary of the invention
The purpose of the present invention is exactly to be directed to the demand of the deficiency and practical application of existing research, and design and provide a kind of tool There is the fluorine silicone encapsulant of self-defoaming function.It is to use trifluompropyl methyl polysiloxane for base rubber, is with acicular titanium dioxide Defoaming and reinforced filling are with dibutyl tin dilaurate using di-iron trioxide as heat-resistant agent, using containing hydrogen silicone oil as vulcanizing agent The dehydrogenation type fluorine silicone encapsulant of catalyst preparation, the purpose is to prepare the fluorine silicone encapsulant with good high temperature resistant oil resistance, It can satisfy the demand of the motor part sealing and electric appliance encapsulating of aircraft, automobile.
The technical scheme is that:
A kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant, it is characterised in that: it is by base cream and vulcanizing agent two A component mixes, the component proportion of base cream and vulcanizing agent are as follows: base cream 99%, vulcanizing agent 1%:
The component proportion of the base cream are as follows:
The liquid fluorosilicone rubber is using hydroxy-end capped trifluompropyl methyl polysiloxane, and viscosity exists Between 20Pa.s-82Pa.s；The titanium dioxide filler be it is needle-shaped, draw ratio be 10:1 to 25:1.
The silica flour granular size is between 0.2 micron -2 microns.
The purity of the di-iron trioxide is between 98%-99.5%.
The dibutyl tin dilaurate trade mark is D-20.
The vulcanizing agent is containing hydrogen silicone oil.
The hydrogen content of the containing hydrogen silicone oil is 0.8%-1.6%.
The preparation method of the self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant:
Base cream is refined using following methods first: each component in base paste formulation being weighed in proportion, by weighed material It is uniformly mixed, is ground 3~5 times using three-roll grinder and form uniform paste, base cream and vulcanizing agent will be prepared by 99:1's Ratio ingredient is uniformly mixed.
The invention has the following advantages over the prior art:
1, self-defoaming formula technique is used, so that homogeneous after sealant vulcanization, performance is stablized.
2, it uses liquid trifluompropyl methyl polysiloxane and prepares dehydrogenation type sealant for liquid raw rubber,
With good heatproof oil resistance.
Specific embodiment
Technical solution of the present invention is further described below with reference to embodiment:
The each component of sealant and its dosage are as shown in table 1 in technical solution of the present invention implementation.Each serial number generation in table 1 A kind of embodiment of sealant of table, wherein serial number 1-3# is experimental example (using acicular titanium dioxide as filler), and 4-6# is pair Than embodiment (using ordinary titanium dioxide as filler).The performance test value of embodiment is as shown in table 2.With serial number 1# in table 1 Implementation for, the step of preparation method of sealant, is as follows:
(1) preparation of base cream: weigh 100 parts of liquid fluorosilicone rubbers (viscosity 20Pa.s), 60-100 parts of acicular titanium dioxides, 4 parts of di-iron trioxides, 10 parts of silica flours, 0.3 part of dibutyl tin dilaurate are kneaded 5 times with three-roll grinder and are uniformly mixed；
(2) preparation of vulcanizing agent: weighing 0.8 part of containing hydrogen silicone oil, and isolation moisture saves；
(3) vulcanizing agent: being added in base cream by the preparation of sealant in 100: 0.8 ratio, is pre-mixed, is then used by hand Three-roll grinder is kneaded 3 times and is uniformly mixed, and then prepares test test piece according to respective standard.Wherein self-defoaming inhales dehydrogenation type fluorine silicon The mechanical property of sealant is tested according to national standard GB/T528-2009, and density measurement is tested according to GB/T 6343-2009.
From table 2 it can be seen that self-defoaming dehydrogenation type fluorine silicone encapsulant of the invention uses the conduct of acicular titanium dioxide filler After defoaming agent, compared with ordinary titanium dioxide is as the fluorine silicone encapsulant performance of filler, porosity decline, heat-resisting oil resistance is mentioned It rises obvious.
The combination and dosage of each component in 1 self-defoaming fluorine silicone encapsulant of table formula
Performance after the vulcanization of 2 self-defoaming fluorine silicone encapsulant sealant of table
Above-mentioned sealant is prepared according to base cream and vulcanizing agent weight ratio 99: 1 when in use, is coated or is perfused after mixing It uses, sealant is i.e. curable at room temperature, and solidification while can be with the hydrogen in Self-discharged sulfidation.

Claims (8)

1. a kind of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant, it is characterised in that: it is by base cream and vulcanizing agent two Component mixes, the component proportion of base cream and vulcanizing agent are as follows: base cream 99%, vulcanizing agent 1%:
The component proportion of the base cream are as follows:
The liquid fluorosilicone rubber is using hydroxy-end capped trifluompropyl methyl polysiloxane, and viscosity is in 20Pa.s- Between 82Pa.s；The titanium dioxide filler be it is needle-shaped, draw ratio be 10:1 to 25:1.
2. self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1, it is characterised in that: the quartz Powder particles size is between 0.2 micron -2 microns.
3. self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1, it is characterised in that: three oxygen Change the purity of two iron between 98%-99.5%.
4. self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1, it is characterised in that: the February The dilaurylate trade mark is D-20.
5. self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1, it is characterised in that: the vulcanizing agent For containing hydrogen silicone oil.
6. self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1, it is characterised in that: the Silicon Containing Hydrogen The hydrogen content of oil is 0.8%-1.6%.
7. the preparation method of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as described in claim 1: base cream uses first Following methods refining: each component in base paste formulation being weighed in proportion, weighed material is uniformly mixed, and is ground using three rollers Machine grinds 3~5 times and forms uniform paste, will prepare base cream and vulcanizing agent and is uniformly mixed in the ratio ingredient of 99:1.
8. the preparation method of self-defoaming dehydrogenation type oil-resistant high-temperature fluorine silicone encapsulant as claimed in claim 7: in the base cream Liquid fluorosilicone rubber be using hydroxy-end capped trifluompropyl methyl polysiloxane, viscosity is between 20Pa.s-82Pa.s； The titanium dioxide filler be it is needle-shaped, draw ratio be 10:1 to 25:1.
CN201910787392.3A 2019-08-23 2019-08-23 Self-defoaming and dehydrogenation type oil-resistant high-temperature-resistant fluorine-silicon sealant and preparation method thereof Active CN110452661B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154454A (en) * 2020-01-07 2020-05-15 芜湖福赛尔航空材料股份有限公司 Oil-resistant silicone sealant

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US20060207723A1 (en) * 2005-03-18 2006-09-21 Wacker Chemie Ag Primer for heat-curable silicone elastomers
CN104830072A (en) * 2015-04-24 2015-08-12 北京化工大学 Fluorinated silicone rubber dielectric elastomer composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060207723A1 (en) * 2005-03-18 2006-09-21 Wacker Chemie Ag Primer for heat-curable silicone elastomers
CN104830072A (en) * 2015-04-24 2015-08-12 北京化工大学 Fluorinated silicone rubber dielectric elastomer composite material and preparation method thereof

Non-Patent Citations (2)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154454A (en) * 2020-01-07 2020-05-15 芜湖福赛尔航空材料股份有限公司 Oil-resistant silicone sealant
CN111154454B (en) * 2020-01-07 2022-03-15 芜湖福赛尔航空材料股份有限公司 Oil-resistant silicone sealant

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