CN103980772B - A kind of nitroso-fluoro-elastomers soaker and preparation technology thereof - Google Patents
A kind of nitroso-fluoro-elastomers soaker and preparation technology thereof Download PDFInfo
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- CN103980772B CN103980772B CN201410224344.0A CN201410224344A CN103980772B CN 103980772 B CN103980772 B CN 103980772B CN 201410224344 A CN201410224344 A CN 201410224344A CN 103980772 B CN103980772 B CN 103980772B
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Abstract
The invention provides a kind of nitroso-fluoro-elastomers soaker and preparation technology thereof.By weight, following component is comprised: nitroso-fluoro-elastomers rubber solution 100 parts, cross-linking agent solution 5-10 part, compounding agent solution 0-5 part; Does is the limiting viscosity of described nitroso-fluoro-elastomers rubber 0.01-0.05? dLg
-1, its physical aspect is liquid form, has room temperature flowable.Nitroso-fluoro-elastomers soaker of the present invention with lower molecular weight, have can the nitroso-fluoro-elastomers polymkeric substance of Room temperature Mobil form for raw material, for the matrix contacting strong acid, highly basic, strong oxidizer and other chemical reagent medium provides barrier propterty, can be used for the numerous areas such as aerospace, chemical industry, electronics and new forms of energy.
Description
Technical field
The invention belongs to organic fluorine material technical field, be specifically related to a kind of nitroso-fluoro-elastomers soaker and preparation technology thereof.
Background technology
Nitroso-fluoro-elastomers (NitrosoRubber is called for short NR) is the high molecular polymer obtained by nitroso-group trifluoromethane, tetrafluoroethylene, the copolymerization of sulfuration point (or cross-linking set) integrated low-temperature.NR high polymer main chain half is carbon-carbon bond (-C-C-), and second half is nitrogen-oxygen bond (-N-O-), and be connected with carbon atom be all fluorine atom, there is good chemical stability; The resistance to low temperature of the nitrogen oxygen chain link imparting rubber excellence that main chain is a large amount of; NR fluorine content is high, and again not containing c h bond, the gas energy knock down the flame of releasing during Pintsch process, even if therefore NR also can not burn in pure oxygen; Good heat resistance, life-time service temperature reaches 180 DEG C.Nitroso-fluoro-elastomers, due to its special powerful oxidation corrosion resistance medium and resistance to low temperature, is the indispensable sealing material of field of aerospace, also has important use at chemical industry, electronics and new energy field.
201310699931.0, the application for a patent for invention that name is called " preparation method of a kind of elastomeric material and preparation method and sealing member ", discloses a kind of low temperature resistant, resistance to N
2o
4elastomeric material of medium and preparation method thereof.This elastomeric material comprises according to moiety and parts by weight: carboxyl nitrsofluoro rubber rubber 90 ~ 100 parts, trifluoracetic acid chromium 0.4 ~ 0.8 part, chromium trifluoride 0.2 ~ 0.5 part, white carbon black 15 ~ 25 parts.This patent is the application that the viton of solid form is processed as sealing product, and can not be used for the preparation of non-regular shape sealing product, product form is single, cannot meet the product demand of soaker.
201310133404.3, name is called the application for a patent for invention of " a kind of nitroso-fluoro-elastomers solution polymerization process ", disclose a kind of nitroso-fluoro-elastomers solution polymerization process, it in dichloromethane solvent, carries out low temperature copolymerization with nitroso-group trifluoromethane, tetrafluoroethylene, cure site monomer, synthesize viton by molecular chain transfer agent telo merization, polymerizable obtains the liquid form nitroso-fluoro-elastomers from solid form to different dynamic viscosity.But this patent is only limitted to the preparation of nitroso-fluoro-elastomers rubber, the application of liquid towards nitroso-fluoro-elastomers is not furtherd investigate.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of nitroso-fluoro-elastomers soaker and preparation technology thereof.With lower molecular weight, have and the nitroso-fluoro-elastomers polymkeric substance of Room temperature Mobil form can form soaker for raw material, for the matrix contacting strong acid, highly basic, strong oxidizer and other chemical reagent medium provides barrier propterty, can be used for the numerous areas such as aerospace, chemical industry, electronics and new forms of energy.
For achieving the above object, the present invention adopts following technical scheme:
A kind of nitroso-fluoro-elastomers soaker, is characterized in that: by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, cross-linking agent solution 5-10 part, compounding agent solution 0-5 part; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.05dLg
-1, its physical aspect is liquid form, has room temperature flowable.
Preferably, the limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.02dLg
-1, low-molecular-weight nitroso-fluoro-elastomers rubber can provide better wetting property and coating.
The massfraction 5-40% of described nitroso-fluoro-elastomers rubber solution, advantage nitroso rubber can be made fully to dissolve in a solvent in this concentration range, is also convenient to realize effectively flooding and applying to matrix simultaneously.
Described cross-linking agent solution and the massfraction of compounding agent solution are 10%, and be convenient to linking agent and auxiliary agent at relatively suitable weightometer weight range, solvent plays diluting effect, be beneficial to evenly mixture.
Described linking agent is the one or any two or more combination in organic multicomponent amine, low molecular polyether amine, aziridine, polycarbodiimide.
The number-average molecular weight of described low molecular polyether amine is 200-500.
In body series, above linking agent is proportionally objective composition with liquid rubber solution by simply stirring mixture, composition can under room temperature mild conditions dip forming.The linking agent selected and the composition that forms of liquid nitroso-fluoro-elastomers have facilitate easy-to-use, the feature of room temperature immersion curing molding, the cladding formed at article surface can be the protective coating that processed product provides the mediums such as strong acid, highly basic, strong oxidizer.
Described auxiliary agent is liquid, is the combination of a kind of in promotor, flow agent or two kinds.
Described nitroso-fluoro-elastomers rubber is with nitroso-group trifluoromethane, tetrafluoroethylene, cure site monomer for polymerized unit, by introducing molecular chain transfer agent in polymerization system, and carries out the high molecular polymer that low temperature copolymerization obtains under methylene dichloride exists.
Preferably, the mol ratio of described nitroso-group trifluoromethane, tetrafluoroethylene, cure site monomer is 45-49.5:50.0-55.5:0.5-2.5.
Preferably, the consumption of described molecular chain transfer agent is the 3-3.5% of cure site monomer, nitroso-group trifluoromethane, tetrafluoroethylene three kinds of total monomer weights.The consumption of molecular chain transfer agent controls within the scope of this, and its transferance is convenient to composite character viscosity at 0.01-0.02dLg
-1rubber.
The preparation technology of nitroso-fluoro-elastomers soaker of the present invention, concrete steps are as follows:
Nitroso-fluoro-elastomers rubber is dissolved in solvent F113 with the mass concentration of 5-40% and is mixed with solution, as component A by A;
Linking agent and auxiliary agent are dissolved in solvent using the mass concentration of 10% and are mixed with solution as B component by B respectively;
C A, B component mix in proportion and namely can be used as steeping fluid for matrix process.
Beneficial effect of the present invention is:
1, soaker of the present invention with lower molecular weight, have and the nitroso-fluoro-elastomers polymkeric substance of Room temperature Mobil form can form soaker for raw material, for the matrix contacting strong acid, highly basic, strong oxidizer and other chemical reagent medium provides barrier propterty, can be used for the numerous areas such as aerospace, chemical industry, electronics and new forms of energy.
2, the linking agent selected of the present invention and the composition that forms of liquid nitroso-fluoro-elastomers have facilitate easy-to-use, the feature of room temperature immersion curing molding, the cladding formed at article surface can be the protective coating that processed product provides the mediums such as strong acid, highly basic, strong oxidizer.
3, the consumption of molecular chain transfer agent controls at 3-3.5% by the present invention, and its transferance is convenient to composite character viscosity at 0.01-0.02dLg
-1rubber.Obtain low-molecular-weight nitroso-fluoro-elastomers rubber and better wetting property and coating can be provided.Be specially adapted to the preparation of soaker, good barrier propterty can be provided for matrix.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, cross-linking agent solution 5 parts, compounding agent solution 1 part; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01dLg
-1, its physical aspect is liquid form, has room temperature flowable.
Embodiment 2
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, organic multicomponent amine aqueous solution 10 parts, flow agent solution 3 parts, accelerator solution 2 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.05dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 40%.
Embodiment 3
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, low molecular polyether amine aqueous solution 6 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.02dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 5%.
The massfraction of described organic multicomponent amine aqueous solution is 10%.
Embodiment 4
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, aziridine solution 7 parts, flow agent solution 2 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.03dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 20%.
Described aziridine solution and the massfraction of flow agent solution are 10%.
Embodiment 5
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, polycarbodiimide solution 7 parts, accelerator solution 3 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.03dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 30%.
Described polycarbodiimide solution and the massfraction of accelerator solution are 10%.
Embodiment 6
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, polycarbodiimide solution 5 parts, aziridine solution 3 parts, flow agent solution 2 parts, accelerator solution 2 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.04dLg
-1, its physical aspect is liquid form, has room temperature flowable.
Described nitroso-fluoro-elastomers rubber solution to be massfraction be 22% nitroso-fluoro-elastomers rubber solution.
Described polycarbodiimide solution and the massfraction of aziridine solution are 10%.
Described flow agent solution and the massfraction of accelerator solution are 10%.
Embodiment 7
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, low molecular polyether amine aqueous solution 5 parts, aziridine solution 4 parts, flow agent solution 2 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.015dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 25%.
Described low molecular polyether amine aqueous solution and the massfraction of aziridine solution are 10%.
The massfraction of described flow agent solution is 10%.
Embodiment 8
A kind of nitroso-fluoro-elastomers soaker, by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, aziridine solution 6 parts, accelerator solution 3 parts; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.018dLg
-1, its physical aspect is liquid form, has room temperature flowable.
The massfraction of described nitroso-fluoro-elastomers rubber solution is 15%.
Described aziridine solution and the massfraction of accelerator solution are 10%.
Embodiment 9
Nitroso-fluoro-elastomers rubber of the present invention is with nitroso-group trifluoromethane, tetrafluoroethylene, cure site monomer for polymerized unit, by introducing molecular chain transfer agent in polymerization system, and carries out the high molecular polymer that low temperature copolymerization obtains under methylene dichloride exists.
Embodiment 10
The embodiment of the present embodiment is substantially the same manner as Example 9, on this basis:
The consumption of described molecular chain transfer agent be cure site monomer, nitroso-group trifluoromethane, tetrafluoroethylene three kinds of total monomer weights 3%.
Embodiment 11
The embodiment of the present embodiment is substantially the same manner as Example 9, on this basis:
The consumption of described molecular chain transfer agent be cure site monomer, nitroso-group trifluoromethane, tetrafluoroethylene three kinds of total monomer weights 3.2%.
Embodiment 12
The embodiment of the present embodiment is substantially the same manner as Example 9, on this basis:
The consumption of described molecular chain transfer agent be cure site monomer, nitroso-group trifluoromethane, tetrafluoroethylene three kinds of total monomer weights 3.5%.
Cure site monomer of the present invention is the one or more kinds of combinations in γ-Trifluoronitrosomethane and Nitrosoperfluorobutyric acid, γ-Trifluoronitrosomethane and Nitrosoperfluorobutyric acid methyl esters, vinylformic acid, trifluoropropyl olefin(e) acid, trifluoropropyl e pioic acid methyl ester.
Molecular chain transfer agent described in this is the one or more kinds of combinations of ether compound, halogen simple substance, flourohalocarbon compound, oxynitrides, nitroxyl free radical trapping agent, two sulfur ester.
Embodiment 13
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A by nitroso-fluoro-elastomers rubber with 40% mass concentration be dissolved in solvent F113 and be mixed with solution, as component A;
B linking agent and auxiliary agent are dissolved in solvent using the mass concentration of 10% respectively and are mixed with solution as B component;
C A, B component mix and namely can be used as steeping fluid for matrix process.
Embodiment 14
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A by nitroso-fluoro-elastomers rubber with 20% mass concentration be dissolved in solvent F113 and be mixed with solution, as component A;
B linking agent is dissolved in solvent using the mass concentration of 10% respectively and is mixed with solution as B component;
C A, B component mix and namely can be used as steeping fluid for matrix process.
Embodiment 15
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A by nitroso-fluoro-elastomers rubber with 25% mass concentration be dissolved in solvent F113 and be mixed with solution, as component A;
B linking agent and auxiliary agent are dissolved in solvent using the mass concentration of 10% respectively and are mixed with solution as B component;
C A, B component mix and namely can be used as steeping fluid for matrix process.
Embodiment 16
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A by nitroso-fluoro-elastomers rubber with 5% mass concentration be dissolved in solvent F113 and be mixed with solution, as component A;
B linking agent and auxiliary agent are dissolved in solvent using the mass concentration of 10% respectively and are mixed with solution as B component;
C A, B component mix and namely can be used as steeping fluid for matrix process.
Treat that solvent volatilizes naturally, then dipping, coat can be obtained with suitable aftertreatment (as natural air drying, baking, hot-air blowing etc.), realize the protection to matrix.
Embodiment 17
By 30 parts of liquid carboxyl nitrsofluoro rubbers, (viscosity is 0.01/dLg
-1acid content 4.5mol%, kinetic viscosity is 28Pa.s) be dissolved in 70 parts of F113 be formulated as mass concentration be the solution of 30% as component A, aziridines linking agent (tetramethylolmethane-three (3-'-aziridino) acrylate) is formulated as the 10% mass concentration aqueous solution as B component.It is 100:5-10 mixture according to parts by weight that A, B measure component, for polytetrafluoroethylglass glass cloth dipping (also can apply) process after abundant stirring and evenly mixing, processes 4h and obtain processing impregnated cloth after solvent volatilizes naturally in 50 DEG C of air-flows.Impregnated cloth is cut into small pieces, and being soaked in concentration is that 98% vitriol oil processes 30 days at ambient temperature, and take out observation surface film and do not change, impregnated cloth rate of mass reduction, lower than 8%, shows and has good tolerance to the vitriol oil.
Embodiment 18
By 30 parts of liquid carboxyl nitrsofluoro rubbers, (viscosity is 0.01/dLg
-1, acid content 4.5mol%, kinetic viscosity is 28Pa.s) be dissolved in 70 parts of F113 be formulated as mass concentration be the solution of 30% as component A, polymine (number-average molecular weight is 600) is formulated as 10% mass concentration ethanolic soln as B component.It is 100:5-10 mixture according to parts by weight that A, B measure component, for polytetrafluoroethylglass glass cloth dipping (also can apply) process after abundant stirring and evenly mixing, processes 4h and obtain processing impregnated cloth after solvent volatilizes naturally in 50 DEG C of air-flows.Impregnated cloth is cut into small pieces, is soaked in 65% concentrated nitric acid and processes 30 days at ambient temperature, take out observation surface film and do not change, impregnated cloth rate of mass reduction, lower than 5%, shows and has good tolerance to nitric acid.
Embodiment 19
The synthesis of liquid nitroso-fluoro-elastomers rubber
Be evacuated after stainless steel polymeric kettle nitrogen replacement, in chuck, the ethanol of logical circulation-70 DEG C, cold medium, is chilled to-60 DEG C by empty still; Utilize the vacuum state of polymeric kettle, add γ-Trifluoronitrosomethane and Nitrosoperfluorobutyric acid 100g, molecular chain transfer agent ether 175g, methylene dichloride 3.5 liters successively with suction; Start polymeric kettle to stir, continue the cold medium of logical circulation in chuck, under still temperature control is lower than-45 DEG C of states, gas phase adds nitroso-group trifluoromethane 1.95kg; Still temperature adds tetrafluoroethylene 2.38kg lower than gas phase under-50 DEG C of conditions.
Polyreaction, with after 18 hours, is opened still separatory and is extracted methylene chloride and liquid polymer respectively out.Polymkeric substance is through water washing, dehydration, except after the postprocessing working procedures such as low molecule, obtain in yellowish transparent liquid rubber 2.48kg, after tested, base limiting viscosity is 0.06/dLg
-1, acid content 1.36%(mol), kinetic viscosity is 61Pa.s.
The synthesis of liquid nitroso-fluoro-elastomers rubber is see patent application 201310133404.3.
Claims (8)
1. a nitroso-fluoro-elastomers soaker, is characterized in that: by weight, comprises following component: nitroso-fluoro-elastomers rubber solution 100 parts, cross-linking agent solution 5-10 part, compounding agent solution 0-5 part; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.05dLg
-1, its physical aspect is liquid form, has room temperature flowable;
Described linking agent is the one or any two or more combination in organic multicomponent amine, low molecular polyether amine, aziridine, polycarbodiimide.
2. a kind of nitroso-fluoro-elastomers soaker according to claim 1, is characterized in that: the limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.02dLg
-1.
3. a kind of nitroso-fluoro-elastomers soaker according to claim 1, is characterized in that: the massfraction of described nitroso-fluoro-elastomers rubber solution is 5-40%.
4. a kind of nitroso-fluoro-elastomers soaker according to claim 1, is characterized in that: described cross-linking agent solution and the massfraction of compounding agent solution are 10%.
5. a kind of nitroso-fluoro-elastomers soaker according to claim 1, is characterized in that: described auxiliary agent, for liquid, is the combination of a kind of in promotor, flow agent or two kinds.
6. a kind of nitroso-fluoro-elastomers soaker according to claim 1, it is characterized in that: described nitroso-fluoro-elastomers rubber is for polymerized unit with nitroso-group trifluoromethane, tetrafluoroethylene, cure site monomer, by introducing molecular chain transfer agent in polymerization system, and carry out the high molecular polymer that low temperature copolymerization obtains under methylene dichloride exists.
7. a kind of nitroso-fluoro-elastomers soaker according to claim 6, is characterized in that: the consumption of described molecular chain transfer agent is the 3-3.5% of cure site monomer, nitroso-group trifluoromethane, tetrafluoroethylene three kinds of total monomer weights.
8. a kind of nitroso-fluoro-elastomers soaker preparation technology according to claim 1, is characterized in that: concrete steps are as follows:
Nitroso-fluoro-elastomers rubber is dissolved in solvent F113 with the mass concentration of 5-40% and is mixed with solution, as component A by A;
Linking agent and auxiliary agent are dissolved in solvent using the mass concentration of 10% and are mixed with solution as B component by B respectively;
C A, B component mix in proportion and namely can be used as steeping fluid for matrix process.
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| CN110734613B (en) * | 2018-07-19 | 2021-06-29 | 中蓝晨光化工研究设计院有限公司 | Nitroso-fluoro rubber composition and application thereof |
| CN110172172B (en) * | 2019-06-21 | 2021-10-08 | 东易日盛智能家居科技有限公司 | Flame-retardant high polymer material veneering paper and preparation method thereof |
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| US3637814A (en) * | 1968-03-27 | 1972-01-25 | Thiokol Chemical Corp | Liquid nitroso rubber prepolymers |
| US3660367A (en) * | 1968-11-13 | 1972-05-02 | Thiokol Chemical Corp | Nitroso polymers |
| CN102746666A (en) * | 2012-07-18 | 2012-10-24 | 中蓝晨光化工研究设计院有限公司 | Carboxynitrosofluoroelastomer composition with low permanent deformation rate |
| CN103214613A (en) * | 2013-04-17 | 2013-07-24 | 中蓝晨光化工研究设计院有限公司 | Nitrosofluoro rubber solution polymerization process |
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| US3637814A (en) * | 1968-03-27 | 1972-01-25 | Thiokol Chemical Corp | Liquid nitroso rubber prepolymers |
| US3660367A (en) * | 1968-11-13 | 1972-05-02 | Thiokol Chemical Corp | Nitroso polymers |
| CN102746666A (en) * | 2012-07-18 | 2012-10-24 | 中蓝晨光化工研究设计院有限公司 | Carboxynitrosofluoroelastomer composition with low permanent deformation rate |
| CN103214613A (en) * | 2013-04-17 | 2013-07-24 | 中蓝晨光化工研究设计院有限公司 | Nitrosofluoro rubber solution polymerization process |
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