CN103980772A - Nitrosofluoro rubber impregnant and preparation technology thereof - Google Patents
Nitrosofluoro rubber impregnant and preparation technology thereof Download PDFInfo
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- CN103980772A CN103980772A CN201410224344.0A CN201410224344A CN103980772A CN 103980772 A CN103980772 A CN 103980772A CN 201410224344 A CN201410224344 A CN 201410224344A CN 103980772 A CN103980772 A CN 103980772A
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Abstract
The invention provides a nitrosofluoro rubber impregnant and a preparation technology thereof. The nitrosofluoro rubber impregnant comprises the following components by parts by weight: 100 parts of nitrosofluoro raw rubber solution, 5-10 parts of crosslinking agent solution and 0-5 parts of assistant solution, wherein the intrinsic viscosity of the nitrosofluoro raw rubber is 0.01-0.05dLg<-1>, the physical form is a liquid form, and the nitrosofluoro rubber impregnant has room-temperature fluidity. According to the nitrosofluoro rubber impregnant disclosed by the invention, a nitrosofluoro rubber polymer with low molecular weight and flow pattern at room temperature is taken as a raw material, and barrier properties are provided for substrates of contacting a strong acid, a strong base, a strong oxidant and other chemical reagent mediums. Therefore, the nitrosofluoro rubber impregnant can be applied to the fields such as aerospace, chemical engineering, electrons, new energy sources and the like.
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 (Nitroso Rubber is called for short NR) is the high molecular polymer being obtained by nitroso-group trifluoromethane, tetrafluoroethylene, the copolymerization of sulfuration point (or cross-linking set) integrated low-temperature.Half is carbon-carbon bond (C-C-) for NR high polymer main chain, 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 a large amount of nitrogen oxygen chain link of main chain is given the resistance to low temperature of rubber excellence; NR fluorine content is high, again containing c h bond, the gas energy knock down the flame of emitting during Pintsch process, even so NR in pure oxygen, can not burn yet; Good heat resistance, life-time service temperature reaches 180 ℃.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, at chemical industry, electronics and new energy field, also has important use.
201310699931.0, name is called the application for a patent for invention of " 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: 90 ~ 100 parts of carboxyl nitrsofluoro rubber rubbers, 0.4 ~ 0.8 part of trifluoracetic acid chromium, 0.2 ~ 0.5 part of chromium trifluoride, 15 ~ 25 parts of white carbon blacks.This patent is the application that the viton of solid form is processed as sealing product, can not be for the preparation of irregular shape sealing product, and 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 ", a kind of nitroso-fluoro-elastomers solution polymerization process is disclosed, it is in dichloromethane solvent, to carry out low temperature copolymerization with nitroso-group trifluoromethane, tetrafluoroethylene, sulfuration point monomer, by the synthetic viton of molecular chain transfer agent telo merization, polymerizable obtains the liquid form nitroso-fluoro-elastomers from solid form to different dynamic viscosity.But this patent only limits 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.Take lower molecular weight, have can room temperature flow-pattern nitroso-fluoro-elastomers polymkeric substance be that raw material forms soaker, for contacting the matrix of strong acid, highly basic, strong oxidizer and other chemical reagent medium, provide 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 nitroso-fluoro-elastomers soaker, is characterized in that: by weight, comprise following component: 100 parts of nitroso-fluoro-elastomers rubber solution, cross-linking agent solution 5-10 part, compounding agent solution 0-5 part; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.05 dLg
-1, its physical aspect is liquid form, has room temperature flowable.
Preferably, the limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.02 dLg
-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 is can, so that nitroso rubber fully dissolves in solvent, to be also convenient to matrix to realize and effectively flood and apply simultaneously in this concentration range.
Described cross-linking agent solution and the massfraction of compounding agent solution are 10%, are convenient to linking agent and auxiliary agent at a relatively suitable weightometer weight range, and solvent plays diluting effect, is beneficial to more uniformly and is mixed.
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 mixed as objective composition by simple stirring with liquid rubber solution, composition can be under room temperature mild conditions dip forming.The composition of the linking agent of selecting and liquid nitroso-fluoro-elastomers composition have facilitate easy-to-use, the feature of room temperature dipping curing molding, the cladding forming on product 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 that to take nitroso-group trifluoromethane, tetrafluoroethylene, sulfuration point monomer be polymerized unit, by introduce 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, sulfuration point 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 sulfuration point monomer, nitroso-group trifluoromethane, three kinds of total monomer weights of tetrafluoroethylene.The consumption of molecular chain transfer agent is controlled within the scope of this, and its transferance is convenient to composite character viscosity at 0.01-0.02 dLg
-1rubber.
The preparation technology of nitroso-fluoro-elastomers soaker of the present invention, concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with the mass concentration of 5-40% and is mixed with solution, as A component;
B is usingd respectively 10% mass concentration by linking agent and auxiliary agent and is dissolved in solvent and is mixed with solution as B component;
C A, B component mix in proportion and can be used as steeping fluid and process for matrix.
Beneficial effect of the present invention is:
1, soaker of the present invention take lower molecular weight, have can room temperature flow-pattern nitroso-fluoro-elastomers polymkeric substance be that raw material forms soaker, for contacting the matrix of strong acid, highly basic, strong oxidizer and other chemical reagent medium, provide barrier propterty, can be used for the numerous areas such as aerospace, chemical industry, electronics and new forms of energy.
The composition of the linking agent that 2, the present invention selects and liquid nitroso-fluoro-elastomers composition have facilitate easy-to-use, the feature of room temperature dipping curing molding, the cladding forming on product surface can be the protective coating that processed product provides the mediums such as strong acid, highly basic, strong oxidizer.
3, the present invention is controlled at 3-3.5% by the consumption of molecular chain transfer agent, and its transferance is convenient to composite character viscosity at 0.01-0.02 dLg
-1rubber.Obtain low-molecular-weight nitroso-fluoro-elastomers rubber better wetting property and coating can be provided.Be specially adapted to the preparation of soaker, can provide good barrier propterty for matrix.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
A nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 5 parts of cross-linking agent solutions, 1 part of compounding agent solution; 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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 10 parts of organic multicomponent amine aqueous solutions, 3 parts of flow agent solution, 2 parts of accelerator solutions; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.05 dLg
-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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 6 parts of low molecular polyether amine aqueous solutions; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.02 dLg
-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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 7 parts of aziridine solution, 2 parts of flow agent solution; 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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 7 parts of polycarbodiimide solution, 3 parts of accelerator solutions; 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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 5 parts of polycarbodiimide solution, 3 parts of aziridine solution, 2 parts of flow agent solution, 2 parts of accelerator solutions; 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 is that massfraction is 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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 5 parts of low molecular polyether amine aqueous solutions, 4 parts of aziridine solution, 2 parts of flow agent solution; 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 nitroso-fluoro-elastomers soaker, by weight, comprises following component: 100 parts of nitroso-fluoro-elastomers rubber solution, 6 parts of aziridine solution, 3 parts of accelerator solutions; 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 that to take nitroso-group trifluoromethane, tetrafluoroethylene, sulfuration point monomer be polymerized unit, by introduce 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 is 3% of a sulfuration point monomer, nitroso-group trifluoromethane, three kinds of total monomer weights of tetrafluoroethylene.
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 is 3.2% of a sulfuration point monomer, nitroso-group trifluoromethane, three kinds of total monomer weights of tetrafluoroethylene.
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 is 3.5% of a sulfuration point monomer, nitroso-group trifluoromethane, three kinds of total monomer weights of tetrafluoroethylene.
Sulfuration point 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 olefin(e) acid methyl esters.
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 esters.
Embodiment 13
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with 40% mass concentration and is mixed with solution, as A component;
B linking agent and auxiliary agent are usingd respectively 10% mass concentration and are dissolved in solvent and are mixed with solution as B component;
C A, B component mix and can be used as steeping fluid and process for matrix.
Embodiment 14
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with 20% mass concentration and is mixed with solution, as A component;
B linking agent is usingd respectively 10% mass concentration and is dissolved in solvent and is mixed with solution as B component;
C A, B component mix and can be used as steeping fluid and process for matrix.
Embodiment 15
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with 25% mass concentration and is mixed with solution, as A component;
B linking agent and auxiliary agent are usingd respectively 10% mass concentration and are dissolved in solvent and are mixed with solution as B component;
C A, B component mix and can be used as steeping fluid and process for matrix.
Embodiment 16
Nitroso-fluoro-elastomers soaker preparation technology of the present invention, concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with 5% mass concentration and is mixed with solution, as A component;
B linking agent and auxiliary agent are usingd respectively 10% mass concentration and are dissolved in solvent and are mixed with solution as B component;
C A, B component mix and can be used as steeping fluid and process for matrix.
Treat that solvent volatilizes naturally, then can obtain dipping, coat 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 4.5 mol %, kinetic viscosity is 28Pa.s) be dissolved in 70 parts of F113 be formulated as mass concentration be 30% solution as A component, aziridines linking agent (tetramethylolmethane-tri-(3-'-aziridino) acrylate) is formulated as to the 10% mass concentration aqueous solution as B component.A, B amount component is that 100:5-10 is mixed according to parts by weight, fully after stirring and evenly mixing, for polytetrafluoroethylglass glass cloth is flooded to (also can apply), processes, and processes 4h and obtain processing impregnated cloth after solvent volatilizes naturally in 50 ℃ of air-flows.Impregnated cloth is cut into small pieces, and being soaked in concentration is that 98% vitriol oil is processed 30 days at ambient temperature, takes out observation surface film and does not change, and impregnated cloth rate of mass reduction, lower than 8%, shows the vitriol oil is had to good tolerance.
Embodiment 18
By 30 parts of liquid carboxyl nitrsofluoro rubbers, (viscosity is 0.01/dLg
-1, acid content 4.5 mol %, kinetic viscosity is 28Pa.s) be dissolved in 70 parts of F113 be formulated as mass concentration be 30% solution as A component, polymine (number-average molecular weight is 600) is formulated as to 10% mass concentration ethanolic soln as B component.A, B amount component is that 100:5-10 is mixed according to parts by weight, fully after stirring and evenly mixing, for polytetrafluoroethylglass glass cloth is flooded to (also can apply), processes, and processes 4h and obtain processing impregnated cloth after solvent volatilizes naturally in 50 ℃ of air-flows.Impregnated cloth is cut into small pieces, is soaked in 65% concentrated nitric acid and processes at ambient temperature 30 days, take out observation surface film and do not change, impregnated cloth rate of mass reduction, lower than 5%, shows nitric acid is had to good tolerance.
Embodiment 19
Synthesizing of liquid nitroso-fluoro-elastomers rubber
By stainless steel polymeric kettle, with being evacuated after nitrogen replacement, the ethanol of cold medium-70 of logical circulation ℃, is chilled to-60 ℃ by empty still in chuck; Utilize the vacuum state of polymeric kettle, with suction, add successively 3.5 liters of γ-Trifluoronitrosomethane and Nitrosoperfluorobutyric acid 100g, molecular chain transfer agent ether 175g, methylene dichloride; Start polymeric kettle and stir, in chuck, continue the cold medium of logical circulation, still temperature control lower than-45 ℃ of states under gas phase add nitroso-group trifluoromethane 1.95kg; Still temperature adds tetrafluoroethylene 2.38kg lower than gas phase under-50 ℃ of conditions.
Polyreaction, with after 18 hours, is opened still separatory and is extracted respectively methylene chloride and liquid polymer out.Polymkeric substance through water washing, dehydration, except postprocessing working procedures such as low molecules after, obtain being 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.
Synthesizing referring to patent application 201310133404.3 of liquid nitroso-fluoro-elastomers rubber.
Claims (9)
1. a nitroso-fluoro-elastomers soaker, is characterized in that: by weight, comprise following component: 100 parts of nitroso-fluoro-elastomers rubber solution, cross-linking agent solution 5-10 part, compounding agent solution 0-5 part; The limiting viscosity of described nitroso-fluoro-elastomers rubber is 0.01-0.05 dLg
-1, its physical aspect is liquid form, has room temperature flowable.
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 0.01-0.02 dLg
-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 linking agent is the one or any two or more combination in organic multicomponent amine, low molecular polyether amine, aziridine, polycarbodiimide.
6. a kind of nitroso-fluoro-elastomers soaker according to claim 1, is characterized in that: described auxiliary agent is for liquid, is the combination of a kind of in promotor, flow agent or two kinds.
7. a kind of nitroso-fluoro-elastomers soaker according to claim 1, it is characterized in that: described nitroso-fluoro-elastomers rubber is that to take nitroso-group trifluoromethane, tetrafluoroethylene, sulfuration point monomer be polymerized unit, by introduce molecular chain transfer agent in polymerization system, and under existing, methylene dichloride carries out the high molecular polymer that low temperature copolymerization obtains.
8. a kind of nitroso-fluoro-elastomers soaker according to claim 7, is characterized in that: the consumption of described molecular chain transfer agent is the 3-3.5% of sulfuration point monomer, nitroso-group trifluoromethane, three kinds of total monomer weights of tetrafluoroethylene.
9. a kind of nitroso-fluoro-elastomers soaker preparation technology according to claim 1, is characterized in that: concrete steps are as follows:
A is dissolved in solvent F113 by nitroso-fluoro-elastomers rubber with the mass concentration of 5-40% and is mixed with solution, as A component;
B is usingd respectively 10% mass concentration by linking agent and auxiliary agent and is dissolved in solvent and is mixed with solution as B component;
C A, B component mix in proportion and can be used as steeping fluid and process for matrix.
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| CN110172172A (en) * | 2019-06-21 | 2019-08-27 | 东易日盛智能家居科技有限公司 | A kind of flame retardant type high molecular material decorative paper and preparation method thereof |
| CN110734613A (en) * | 2018-07-19 | 2020-01-31 | 中蓝晨光化工研究设计院有限公司 | nitroso-fluoro rubber composition and its application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110734613A (en) * | 2018-07-19 | 2020-01-31 | 中蓝晨光化工研究设计院有限公司 | nitroso-fluoro rubber composition and its application |
| 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 |
| CN110172172A (en) * | 2019-06-21 | 2019-08-27 | 东易日盛智能家居科技有限公司 | A kind of flame retardant type high molecular material decorative paper and preparation method 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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