CN103483827B - Fire-retardant fluorine silica gel - Google Patents
Fire-retardant fluorine silica gel Download PDFInfo
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- CN103483827B CN103483827B CN201310423138.8A CN201310423138A CN103483827B CN 103483827 B CN103483827 B CN 103483827B CN 201310423138 A CN201310423138 A CN 201310423138A CN 103483827 B CN103483827 B CN 103483827B
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- fire
- retardant
- fluorine
- weight portion
- fluorine silica
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Abstract
The present invention provides a kind of fire-retardant fluorine silica-gel composition, and wherein, described fire-retardant fluorine silica-gel composition includes following component the most in parts by weight: fluorine silicon raw rubber 190～210 weight portion；Described fluorine silicon raw rubber includes that fluorine silicon raw rubber that contents of ethylene is 0.03 ± 0.01% and contents of ethylene are the fluorine silicon raw rubber of 0.2 ± 0.02%, and the part by weight of the two is 1:(0.8～1.2)；Fluorosilicon oil 19～21 weight portion；Vinyl trialkyl oxysilane 1.6 ± 0.05 weight portion；Calcium carbonate 13～17 weight portion；Magnesium hydroxide 75～85 weight portion.The present invention also provides for corresponding fire-retardant fluorine silica gel and purposes.
Description
Technical field
The present invention relates to a kind of fluorosioloxane rubber, relate more specifically to a kind of fire-retardant fluorosioloxane rubber.
Background technology
Fluorosioloxane rubber is a kind of to have excellent oil resistant, solvent resistance, under the conditions of immersion oil, maximum operation (service) temperature up to
180℃.Stability at ambient and elevated temperatures is all fine, can in the range of-50 DEG C～+200 DEG C Long-Time Service, but it does not has
Having anti-flammability, at present, market does not also have production and the sale of fire-retardant fluorine silica gel, the needs for this part bring the biggest
Inconvenience.
Fluorine silica gel itself does not have fire resistance, due to the viscosity of fluorine silica gel, is difficult to mate to general material, coordinates
Come elastic the most poor.
In sum, shortage one in this area has elasticity and anti-flammability, and the fluorosioloxane rubber of the unlikely deterioration of performance own concurrently
And preparation method thereof.
Summary of the invention
The first object of the present invention is that obtaining one has elasticity and anti-flammability, and the fluorine silicon of the unlikely deterioration of performance own concurrently
Rubber composition.
The second object of the present invention is that obtaining one has elasticity and anti-flammability, and the fluorine silicon of the unlikely deterioration of performance own concurrently
Rubber.
The third object of the present invention is that obtaining one has elasticity and anti-flammability, and the fluorine silicon of the unlikely deterioration of performance own concurrently
The preparation method of rubber.
The fourth object of the present invention is that obtaining one has elasticity and anti-flammability, and the fluorine silicon of the unlikely deterioration of performance own concurrently
The purposes of rubber.
In a first aspect of the present invention, it is provided that a kind of fire-retardant fluorine silica-gel composition, wherein, described fire-retardant fluorine silica gel composition
Thing includes following component the most in parts by weight:
Fluorine silicon raw rubber 190～210 weight portion；Described fluorine silicon raw rubber includes the fluorine silicon that contents of ethylene is 0.03 ± 0.01%
Rubber and contents of ethylene are the fluorine silicon raw rubber of 0.2 ± 0.02%, and the part by weight of the two is 1:(0.8～1.2)；
Fluorosilicon oil 19～21 weight portion；
Vinyl trialkyl oxysilane 1.6 ± 0.05 weight portion；
Calcium carbonate 13～17 weight portion；
Magnesium hydroxide 75～85 weight portion.
In a specific embodiment of the present invention, described vinyl trialkyl oxysilane preferably is selected from vinyl trimethoxy
Base silane.
In a specific embodiment of the present invention, possibly together with Methyl-ethylenvinyl gum 3.5～4.5 weight in described component
Amount part.
In a specific embodiment of the present invention, the contents of ethylene of described Methyl-ethylenvinyl gum is 0.08 ±
0.01%。
In a specific embodiment of the present invention, possibly together with filler in described composition.
In a specific embodiment of the present invention, described filler is the white carbon H-5 of 38～42 weight portions, and 38
～42 white carbon N20 of weight portion.
A second aspect of the present invention provides the fire-retardant fluorine silica gel that a kind of fire-retardant fluorine silica-gel composition of the present invention obtains.
A third aspect of the present invention provides the preparation method of a kind of fire-retardant fluorine silica gel of the present invention, including walking as follows
Rapid:
The blend glue stuff of each component of the fluorine silica-gel composition of the present invention is provided；
Described sizing material carries out mixing, obtains mixing uniform sizing material；
Described sizing material post-processes, and obtains described fire-retardant fluorine silica gel.
In a specific embodiment of the present invention, described post processing includes: cut into slices by described mixing uniform sizing material,
Process 90 ± 20 minutes at 175 ± 10 DEG C again, obtain described fire-retardant fluorine silica gel.
A fourth aspect of the present invention provides a kind of fire-retardant fluorine silica gel of the present invention in the range of-50 DEG C～+200 DEG C
Application.
Detailed description of the invention
The present inventor is through extensively in-depth study, by improving preparation technology, it is thus achieved that one has superior elasticity concurrently
Fluorosioloxane rubber with fire resistance.Complete the present invention on this basis.
The technology design of the present invention is as follows:
Fluorine silica gel itself does not have fire resistance, due to the viscosity of fluorine silica gel, is difficult to mate to general material, coordinates
Come elastic the most poor.To this end, inventor is through great many of experiments, find specific fluorine silicon raw rubber combination, specific fire retardant, specific
The cooperation of additive is so that its anti-flammability, elasticity all reach necessary requirement, and performance is unlikely to deterioration ,-50 DEG C～+
All can apply well for 200 DEG C.
In the present invention, term " contains " or " including " represents that various composition can be applied to mixture or the group of the present invention together
In compound.Therefore, term " mainly by ... composition " and " consist of " be included in term and " contain " or in " including ".
" alkyl " as used herein, described, except as otherwise noted, refers to the straight chain containing 1-4 carbon atom or props up
Alkane.The preferably alkane containing 1-2 carbon atom, such as, alkyl includes but not limited to methyl, ethyl.
Hereinafter it is described in detail to various aspects of the present invention:
Fire-retardant fluorine silica-gel composition
The present invention provides a kind of fire-retardant fluorine silica-gel composition, and wherein, described fire-retardant fluorine silica-gel composition includes as follows with weight
The component of amount part meter:
Fluorine silicon raw rubber 190～210 weight portion；Described fluorine silicon raw rubber includes the fluorine silicon that contents of ethylene is 0.03 ± 0.01%
Rubber and contents of ethylene are the fluorine silicon raw rubber of 0.2 ± 0.02%, and the part by weight of the two is 1:(0.8～1.2)；
Fluorosilicon oil 19～21 weight portion；
Vinyl trialkyl oxysilane 1.6 ± 0.05 weight portion；
Calcium carbonate 13～17 weight portion；
Magnesium hydroxide 75～85 weight portion.
The definition of described " fluorine silicon raw rubber " is well known by persons skilled in the art.Such ashttp:// Wenku.baidu.com/view/893d71c258f5f61fb73666d8.html (access on September 12nd, 2013)Record
Described in " synthesis of fluorine silicon raw rubber and crosslinking feature " (Zhejiang chemical industry, the 2nd phase of volume 38 in 2007 reach et al. recklessly)；But
It is not limited to this.Described " fluorine silicon raw rubber " can be obtained to those skilled in the art easily by be commercially available.
The contents of ethylene of described " fluorine silicon raw rubber " can pass through iodometric determination.Such as " fluorosioloxane rubber medium vinyl contains
The mensuration of amount " (model security personnel etc., China Synthetic Rubber Industry, volume 1981,4, page 444～446).
Inventor finds, the cooperation between the fluorine silicon raw rubber of described specific contents of ethylene, and (improves glue with fluorosilicon oil
The processing characteristics of material), the vinyl trialkyl oxysilane crosslink density of sizing material (improve), magnesium hydroxide (screened a large amount of fire-retardant
After agent selected), calcium carbonate (as filler, and improving its mobility) coordinate, successfully obtain and there is good flame resistance, elasticity is also
The most excellent, and the fluorosioloxane rubber of stable performance (can in the range of-50 DEG C～+200 DEG C Long-Time Service).
In a preferred embodiment, described vinyl trialkyl oxysilane preferably is selected from vinyltrimethoxy silane.
Inventor finds, when in described formula containing vinyltrimethoxy silane, the crosslinking that can improve sizing material is close
Degree.
In a preferred embodiment, possibly together with Methyl-ethylenvinyl gum 3.5～4.5 weight portion in described component.
Inventor finds, when in described formula containing Methyl-ethylenvinyl gum, can improve the performance of the processing of sizing material.
In a preferred embodiment, the contents of ethylene of described Methyl-ethylenvinyl gum is 0.08 ± 0.01%.
In a preferred embodiment, possibly together with filler in described composition.In a preferred embodiment, described
Filler is the white carbon H-5 of 38～42 weight portions, and the white carbon N20 of 38～42 weight portions.
Preparation method
The present invention also provides for the preparation method of a kind of fire-retardant fluorine silica gel of the present invention, and it comprises the steps:
The blend glue stuff of the component described in composition of the present invention is provided；
Described sizing material carries out mixing, obtains mixing uniform sizing material；
Described sizing material post-processes, and obtains described fire-retardant fluorine silica gel.
In a preferred embodiment, described post processing includes: cut into slices by described mixing uniform sizing material, then 175
Process 90 ± 20 minutes at ± 10 DEG C, obtain described fire-retardant fluorine silica gel.
Fire-retardant fluorine silica gel of the present invention can be in the application in the range of-50 DEG C～+200 DEG C.
Preferred embodiment
Fluorine silicon raw rubber contents of ethylene 0.03 ± 0.01%100 ± 5 parts, 0.2 ± 0.02%100 ± 5 parts, fluorosilicon oil 20 ± 1
Part, Methyl-ethylenvinyl gum vinyl 0.08% ± 0.014 ± 0.5 part, white carbon H-540 ± 2 part, white carbon N2040 ± 2 part,
Vinyltrimethoxy silane 1.6 ± 0.05 parts, 15 ± 2 parts of calcium carbonate, magnesium hydroxide 80 ± 5 parts.
As no specific instructions, the various raw materials of the present invention all can be by being commercially available；Or the routine side according to this area
Method prepares.Unless otherwise defined or described herein, all specialties used herein are ripe with art technology with scientific words
The meaning that white silk personnel are familiar with is identical.The most any method similar or impartial to described content and material all can be applicable to this
In inventive method.
Other aspects of the present invention, due to this disclosure, are apparent to those skilled in the art
's.
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, generally marks according to country
Quasi-mensuration.If there is no corresponding national standard, then according to general international standard, normal condition or built according to manufacturer
The condition of view is carried out.Unless otherwise indicated, the most all of number is weight portion, and all of percentage is weight percentage, institute
The polymer molecular weight stated is number-average molecular weight.
Unless otherwise defined or described herein, all specialties used herein and scientific words and the skilled people of art technology
The meaning that member is familiar with is identical.The most any method similar or impartial to described content and material all can be applicable to the present invention
In method.
Embodiment 1 (preferred embodiment)
Fluorine silicon raw rubber contents of ethylene 0.03%100 part, 0.2%100 part, fluorosilicon oil 20 parts, Methyl-ethylenvinyl gum ethene
0.08%4 part of base, white carbon H-540 part, white carbon N2040 part, vinyltrimethoxy silane 1.6 parts, 15 parts of calcium carbonate, hydrogen
80 parts of magnesia.
Technique is as follows:
1, rubber is put bag roller on a mill until, is initially charged white carbon and silicone oil, add calcium carbonate and magnesium hydroxide and
Vinyltrimethoxy silane adds, point 3-4 addition, stirs several times more, and material plays 6 triangle bags, by rubber compounding after adding
Uniformly.
2, the sizing material mixed goes out the thin slice of 3-4mm, puts 175 DEG C × 90min of process in an oven
Fire-retardant rank: reach the UL94V1 of the U.S.
Embodiment 2
Fluorine silicon raw rubber contents of ethylene 0.03%100 part, fluorine silicon raw rubber contents of ethylene 0.2%100 part, fluorosilicon oil 20 parts,
Methyl-ethylenvinyl gum vinyl 0.08%4 part, white carbon H-540 part, white carbon N2040 part, 15 parts of calcium carbonate, magnesium hydroxide
80 parts.
Technique is as follows:
Rubber is put bag roller on a mill until, is initially charged white carbon and silicone oil, add and calcium carbonate and magnesium hydroxide are added,
Dividing 3-4 time to add, stir several times more, material plays 6 triangle bags after adding, and rubber compounding is uniform.
The sizing material mixed goes out the thin slice of 3-4mm, puts 175 DEG C × 90min of process in an oven.
Result display sizing material hardness decreases, and percentage elongation is elongated, and resilience is deteriorated (relative preferred embodiment)
Fire-retardant rank: reach the UL94V1 of the U.S.
Embodiment 3
Fluorine silicon raw rubber contents of ethylene 0.03%100 part, fluorine silicon raw rubber contents of ethylene 0.2%100 part, fluorosilicon oil 20 parts,
Methyl-ethylenvinyl gum vinyl 0.08%4 part, white carbon H-540 part, white carbon N2040 part, VTES
1.6 parts, 15 parts of calcium carbonate, magnesium hydroxide 80 parts.
Technique is as follows:
Rubber is put bag roller on a mill until, is initially charged white carbon and silicone oil, add calcium carbonate, vinyl triethoxyl
Silane, magnesium hydroxide adds, point 4-5 addition, stirs several times more, and material plays 6 triangle bags after adding, and rubber compounding is uniform.
The sizing material mixed goes out the thin slice of 3-4mm, puts 175 DEG C × 90min of process in an oven
Comparative example 1:
Fluorine silicon raw rubber contents of ethylene 0.03%100 part, 0.2%100 part, fluorosilicon oil 20 parts, Methyl-ethylenvinyl gum ethene
0.08%4 part of base, white carbon H-540 part, white carbon N2040 part, vinyltrimethoxy silane 1.6 parts, 15 parts of calcium carbonate, hydrogen
80 parts of aluminum oxide.
Technique is as follows:
Rubber is put bag roller on a mill until, is initially charged white carbon and silicone oil, add calcium carbonate and aluminium hydroxide and second
Thiazolinyl trimethoxy silane adds, point 3-4 addition, stirs several times more, and material plays 6 triangle bags after adding, and rubber compounding is equal
Even.
The sizing material mixed goes out the thin slice of 3-4mm, puts 175 DEG C × 90min of process in an oven
| Sequence number | Detection project name and unit | Testing result | Detection method |
| 1 | Continue your hardness；Degree | 58 | GB/T531.1-2008 |
| 2 | Hot strength；MPA | 4.0 | GB/T528-1998 |
| 3 | Elongation rate of tensile failure | 200 | GB/T528-1998 |
| 4 | Tearing strength (perpendicular type)；KN/m | 15 | GB/T529-2008 |
Sulphur situation of significantly owing worked it out by sizing material, and sizing material coordinates unsuitable for aluminium hydroxide.
Comparative example 2
Fluorine silicon raw rubber contents of ethylene 0.03%100 part, fluorine silicon raw rubber contents of ethylene 0.2%100 part, fluorosilicon oil 20 parts,
Methyl-ethylenvinyl gum vinyl 0.08%4 part, white carbon H-540 part, white carbon N2040 part, vinyltrimethoxy silane
1.6 parts, 15 parts of calcium carbonate
Technique is as follows:
Rubber is put bag roller on a mill until, is initially charged white carbon and silicone oil, add calcium carbonate vinyl trimethoxy
Silane adds, point 3-4 addition, stirs several times more, and material plays 6 triangle bags after adding, and rubber compounding is uniform.
The sizing material mixed goes out the thin slice of 3-4mm, puts 175 DEG C × 90min of process in an oven
Conclusion:
Sizing material does not has fire resistance.During without fire retardant, other physical and mechanical properties increase, but can not meet resistance
The demand of combustion fluorine silica gel.Accordingly, it would be desirable to consider how to add fire retardant, it is unlikely to again so that other hydraulic performance declines simultaneously.
The foregoing is only presently preferred embodiments of the present invention, be not limited to the substantial technological content model of the present invention
Enclosing, the substantial technological content of the present invention is broadly to be defined in the right of application, any technology that other people complete
Entity or method, if with the right of application defined in identical, also or the change of a kind of equivalence, all by
It is considered to be covered by among this right.
The all documents mentioned in the present invention are incorporated as reference the most in this application, just as each document by individually
It is incorporated as with reference to like that.In addition, it is to be understood that after the foregoing having read the present invention, those skilled in the art can be right
The present invention makes various changes or modifications, and these equivalent form of values fall within the application appended claims limited range equally.
Claims (7)
1. a fire-retardant fluorine silica-gel composition, wherein, described fire-retardant fluorine silica-gel composition includes following component the most in parts by weight:
Fluorine silicon raw rubber 190～210 weight portion；Described fluorine silicon raw rubber includes the fluorine silicon raw rubber that contents of ethylene is 0.03 ± 0.01%
It is the fluorine silicon raw rubber of 0.2 ± 0.02% with contents of ethylene, and the part by weight of the two is 1:(0.8～1.2)；
Fluorosilicon oil 19～21 weight portion；
Vinyl trialkyl oxysilane 1.6 ± 0.05 weight portion；
Calcium carbonate 13～17 weight portion；
Magnesium hydroxide 75～85 weight portion.
Fire-retardant fluorine silica-gel composition the most as claimed in claim 1, it is characterised in that described vinyl trialkyl oxysilane is preferred
From vinyltrimethoxy silane.
Fire-retardant fluorine silica-gel composition the most as claimed in claim 1, it is characterised in that possibly together with contents of ethylene in described component
It it is Methyl-ethylenvinyl gum 3.5～4.5 weight portion of 0.08 ± 0.01%.
Fire-retardant fluorine silica-gel composition the most as claimed in claim 1, it is characterised in that possibly together with 38～42 weights in described composition
The white carbon H-5 of amount part, and the white carbon N20 of 38～42 weight portions.
5. the fire-retardant fluorine silica gel that a fire-retardant fluorine silica-gel composition as claimed in claim 1 obtains.
6. the preparation method of a fire-retardant fluorine silica gel as claimed in claim 5, it is characterised in that comprise the steps:
The blend glue stuff of offer component as described in Claims 1 to 4 any one；
Described sizing material carries out mixing, obtains mixing uniform sizing material；
Described sizing material post-processes, and obtains described fire-retardant fluorine silica gel.
7. method as claimed in claim 6, it is characterised in that described post processing includes: cut by described mixing uniform sizing material
Sheet, then process 90 ± 20 minutes at 175 ± 10 DEG C, obtain described fire-retardant fluorine silica gel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310423138.8A CN103483827B (en) | 2013-09-16 | 2013-09-16 | Fire-retardant fluorine silica gel |
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|---|---|---|---|
| CN201310423138.8A CN103483827B (en) | 2013-09-16 | 2013-09-16 | Fire-retardant fluorine silica gel |
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| CN103483827B true CN103483827B (en) | 2016-08-17 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105754353A (en) * | 2016-03-28 | 2016-07-13 | 东莞市亚马电子有限公司 | High-thermal-conductivity silicone rubber and preparation process thereof |
| CN109096776B (en) * | 2018-08-13 | 2021-07-09 | 山东大学 | Catalyst-free fast-curing dealcoholized fluorosilicone rubber and preparation method thereof |
| CN111961347A (en) * | 2020-08-27 | 2020-11-20 | 东莞市利群榕兴高分子科技有限公司 | High-conductivity fluorosilicone rubber composition, preparation method and electromagnetic shielding material |
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| CN102250472A (en) * | 2011-05-18 | 2011-11-23 | 杨福河 | High-performance silicon-based conductive rubber and preparation method thereof |
| CN102410410A (en) * | 2011-07-25 | 2012-04-11 | 北京天元奥特橡塑有限公司 | Inner-fluorin and outer-silicon tube with fire resistance, high and low temperature resistance and oil resistance and preparation method thereof |
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| CN1720291A (en) * | 2002-12-05 | 2006-01-11 | 大金工业株式会社 | Fluorine-containing polymer composition and cured body |
| CN101177486A (en) * | 2007-11-02 | 2008-05-14 | 广东信力特种橡胶制品有限公司 | Method for preparing fluorine silicon rubber base glue |
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