CN107880562A - Expandable flame retardant silicon rubber composite material and preparation method thereof - Google Patents
Expandable flame retardant silicon rubber composite material and preparation method thereof Download PDFInfo
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- CN107880562A CN107880562A CN201711303981.7A CN201711303981A CN107880562A CN 107880562 A CN107880562 A CN 107880562A CN 201711303981 A CN201711303981 A CN 201711303981A CN 107880562 A CN107880562 A CN 107880562A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/327—Aluminium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The present invention is relevant a kind of expandable flame retardant silicon rubber composite material and preparation method thereof, wherein expandable flame retardant silicon rubber composite material includes 100 parts of methyl vinyl silicon kautschuk, 20 30 parts of reinforced filling, 0 20 parts of expansible graphite, 0 20 parts of phosphoric acid salt fire retardant, 24 parts of vulcanizing agent, 46 parts of silicone oil, the material are weight ratio.The silicon rubber composite material of expandable flame retardant of the present invention, makes expandable flame retardant silicon rubber composite material strengthen layer of charcoal intensity during fire-retardant, and application is wider.
Description
Technical field
The present invention relates to a kind of elastomeric material, more particularly to a kind of expandable flame retardant silicon rubber composite material and its preparation side
Method.
Background technology
Silicon rubber is a kind of special polymer using Si-O as main chain, has inorganic in nature and organic nature concurrently, because of its tool
There is the structure of inorganic silicon oxygen bond and side chain organic group (R), be a kind of especially wide elastic polymer material of application, due to
It has specific chemical stability, resistant of high or low temperature, weatherability, an insulating properties, while few cigarette is nontoxic, fuel value in burning
It is low, it is possible to all trades and professions in fields such as military affairs, aviations, being also employed in national economy are applied as special material, such as
Chemical industry, machine-building, weaving papermaking etc..It is the organic of carbochain because its molecular backbone is Si-O structures, therefore with other main chains
Rubber is compared, and the limited oxygen index (LOI) of silicon rubber burning is higher, but despite of that, silicon rubber, which meets naked light, can still continue to fire
Burn, so carrying out fire-retardant research to silicon rubber, to improve its performance very necessary.
The content of the invention
It is an object of the invention to provide a kind of silicon rubber composite material of expandable flame retardant and preparation method thereof, with solution
The problem of existing is stated, expandable flame retardant silicon rubber composite material is strengthened layer of charcoal intensity during fire-retardant, application is wider.
The object of the invention to solve the technical problems is realized using following technical scheme.Carried according to the present invention
The expandable flame retardant silicon rubber composite material gone out, including 100 parts of methyl vinyl silicon kautschuk, reinforced filling 20-30 parts can be swollen
Swollen graphite 0-20 parts, phosphoric acid salt fire retardant 0-20 parts, vulcanizing agent 2-4 parts, silicone oil 4-6 parts, the material are weight ratio.
The purpose of the present invention and solve its technical problem and can also be further achieved by the following technical measures.
Foregoing expandable flame retardant silicon rubber composite material, wherein the reinforced filling be calcium carbonate, white carbon, zinc oxide,
At least one of titanium dioxide.
Foregoing expandable flame retardant silicon rubber composite material, wherein described phosphoric acid salt fire retardant be APP, red phosphorus,
At least one of aluminium triphosphate, diethyl hypo-aluminum orthophosphate, ammonium phosphate salt.
Foregoing expandable flame retardant silicon rubber composite material, wherein the silicone oil is methyl vinyl silicon oil, high activity ethene
At least one of base silicone oil, methyl-silicone oil.
Foregoing expandable flame retardant silicon rubber composite material, wherein the vulcanizing agent is the double (tert-butyl groups of 2,5- dimethyl -2,5-
At least one of peroxy) hexane, 2,4- dichlorides BP or cumyl peroxide.
Foregoing expandable flame retardant silicon rubber composite material, wherein the expansible graphite is 10-20 parts, the phosphoric acid salt
Fire retardant is 10-20 parts.
The preparation method of expandable flame retardant silicon rubber composite material of the present invention, comprises the steps：(1) by 100 parts of methyl second
Alkenyl raw-silastic continuously, 20-30 parts supporting material, 0-20 parts expansible graphite, 0-20 part phosphoric acid salts filler are kneaded uniform；
(2) it is kneaded in the mixture for obtaining 4-6 parts methyl-silicone oil addition step (1) uniform；(3) 2-4 parts vulcanizing agent is added and walked
Suddenly it is well mixed in the mixture that (two) obtain, slice obtains mixing of rubber；(4) by above-mentioned mixing of rubber full cure, it is made
Required test piece.
The preparation method of foregoing expandable flame retardant silicon rubber composite material, wherein the sulfidation 140-170 DEG C,
Carried out under 10-15Mpa pressure, cure time 10-15 minutes.
The preparation method of foregoing expandable flame retardant silicon rubber composite material, wherein the phosphoric acid salt fire retardant is through drying.
The preparation method of foregoing expandable flame retardant silicon rubber composite material, wherein the step (1) and step (2) are double
Carried out in roller kneading machine or banbury.
By above-mentioned technical proposal, the present invention at least has following advantages and beneficial effect：
(1) because expandable flame retardant silicon rubber composite material of the present invention includes methyl vinyl silicon kautschuk, reinforced filling,
Expansible graphite, phosphoric acid salt fire retardant, vulcanizing agent, silicone oil, therefore there is good fire resistance, reinforced filling therein removes
Silicon rubber can be risen outside strengthening action, can also be by diluting combustible concentration, improving silicon rubber intermolecular interaction
Power improves the heat endurance of silicon rubber, plays an important roll to the fire-retardant of silicon rubber, while the present invention with the addition of inflatable stone
Ink, expansible graphite aboundresources, is simple to manufacture, cheap, nontoxic, low cigarette, when it is rapidly heated to more than 220 DEG C
When, it can be expanded hundreds times along the direction of principal axis of crystalline texture, after expanding at high temperature, both form the charcoal source in intumescent system,
Heat insulation layer is formd again, can effectively act as heat-insulating flame-retardant effect, and addition phosphoric acid salt fire retardant also significantly improves later
Layer of charcoal intensity after rubber combustion, further enhances the anti-flammability of silicon rubber, also improves the mechanics of silicon rubber composite material
Performance.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, and
It can be practiced according to the content of specification, and to allow the above and other objects, features and advantages of the present invention can be brighter
It is aobvious understandable, below especially exemplified by preferred embodiment, describe in detail as follows.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Preferred embodiment, to embodiment, feature and its effect of the present invention, describe in detail as after.
Embodiment one
A kind of preparation method of expandable flame retardant silicon rubber composite material of the present invention, comprises the steps：
100 parts of methyl vinyl silicon kautschuks and 30 parts of reinforced filling calcium carbonate are blended 10 points in double roll mill
Clock, it is well mixed, the molecular weight of methyl vinyl silicone rubber therein is more than 500,000；
4 parts of silicone oil is added in double roll mill and continues to be blended, silicone oil selects methyl vinyl silicon oil；
2 parts of vulcanizing agent is added in said mixture and is well mixed, slice obtains mixing of rubber, and vulcanizing agent uses
2,5- dimethyl -2,5- bis(t-butylperoxy)s hexane (is commonly called as double 2,5)；
By above-mentioned mixing of rubber under 160 DEG C, 15Mpa pressure, vulcanize 12 minutes, obtain silicon rubber, performance is carried out to it
Test, during test, silicon rubber is cut into 20 × 20 × 3mm3Cuboid sample, in Muffle furnace 400 DEG C roasting half an hour
After take out, apply the counterweight of different weight to it, the strength definition for bearing 500g counterweights is A, bears the strong of 200-500g counterweights
Spend for B, the strength definition born less than 200g counterweights is C.Its performance is as shown in the table.
Embodiment two
100 parts of methyl vinyl silicon kautschuks and 25 parts of reinforced filling are blended 10 minutes in banbury, wherein
Methyl vinyl silicone rubber molecular weight be more than 500,000, reinforced filling selects zinc oxide；
5 parts of silicone oil is added in above-mentioned banbury and continues to be blended, silicone oil selects high activity vinyl silicone oil；
3 parts of vulcanizing agents are added into mixing in said mixture, and, until well mixed, slice obtains mixing of rubber, above-mentioned sulphur
Agent is using 2,4- dichlorides BP (being commonly called as double 2,4)；
By above-mentioned mixing of rubber under 140 DEG C, 12Mpa pressure, vulcanize 10 minutes, required sample is made, to its progressive
It can test, performance test methods are identical with embodiment one, and its performance is as shown in the table.
Embodiment three
100 parts of methyl vinyl silicon kautschuks and 20 parts of reinforced filling are blended 10 points in double roll mill first
Clock, adding 20 parts of expansible graphites and continue to mix to uniform, the molecular weight of methyl vinyl silicone rubber therein is more than 500,000,
Reinforced filling selects zinc oxide, and expansible graphite is the interlayer that natural flake graphite handles to obtain through chemical reagent such as the concentrated sulfuric acids
Compound, it is black flaky thing, can be hundreds of along the direction of principal axis expansion of crystalline texture when it is rapidly heated to more than 220 DEG C
Times.Because graphite layers adhesion is weak, layer structure is easy to move from other connected structure China and foreign countries, so being occluded in interlayer
Compound can decompose；When graphite is heated, its volume, which can expand rapidly, makes flame suffocate, so as to reach fire-retardant purpose, in fire
In rate of heat release it is very low, weight-loss ratio very little, basic smokeless generation.In addition, it also has the characteristics that nontoxic, pollution-free, inexpensive,
It is adapted to the requirement of present Halogen agent；
6 parts of silicone oil are added in double roll mill and continue to be blended, silicone oil selects methyl-silicone oil；
4 parts of vulcanizing agents are added in said mixture and are blended into well mixed, slice obtains mixing of rubber, above-mentioned vulcanization
Agent uses cumyl peroxide (being commonly called as DCP)；
By above-mentioned mixing of rubber under 170 DEG C, 10Mpa pressure, vulcanize 13 minutes, required sample is made, to its progressive
It can test, performance test methods are identical with embodiment one, and its performance is as shown in the table.
Example IV
100 parts of methyl vinyl silicon kautschuks and 28 parts of reinforced filling zinc oxide are blended 10 points in banbury
Clock, add 10 parts of expansible graphites and be well mixed, add 10 parts of aluminium triphosphates, point of methyl vinyl silicone rubber therein
Son amount is more than 500,000, and aluminium triphosphate ensures its drying property because water imbibition needs to dry 7h at 80 DEG C in an oven by force；
4 parts of silicone oil is added in banbury and continues to be blended, silicone oil selects methyl vinyl silicon oil and high activity
The mixture of vinyl silicone oil；
2 parts of vulcanizing agent is added in said mixture and is well mixed, slice obtains mixing of rubber, and vulcanizing agent uses 2,
5- dimethyl -2,5- bis(t-butylperoxy)s hexane (being commonly called as double 2,5) and 2,4- dichlorides BP (being commonly called as double 2,4)
Mixture；
By above-mentioned mixing of rubber under 160 DEG C, 13Mpa pressure, vulcanize 15 minutes, required sample is made, to its progressive
It can test, performance test methods are identical with embodiment one, and its performance is as shown in the table.
Embodiment five
100 parts of methyl vinyl silicon kautschuks and 30 parts of reinforced filling are blended 10 minutes in double roll mill,
Then add 20 parts of phosphate, the molecular weight of methyl vinyl silicone rubber therein is more than 500,000, reinforced filling from calcium carbonate,
White carbon, zinc oxide, the mixture of titanium dioxide, phosphate are above-mentioned from diethyl hypo-aluminum orthophosphate, the mixture of ammonium phosphate salt
Phosphate ensures its drying property because water imbibition needs to dry 7h at 80 DEG C in an oven by force；
4 parts of silicone oil are added in double roll mill and continue to be blended, silicone oil is from methyl vinyl silicon oil, high activity
The mixture of vinyl silicone oil, methyl-silicone oil；
2 parts of vulcanizing agents are added in said mixture and continue to be well mixed, slice obtains mixing of rubber, and vulcanizing agent uses
Mixing of the 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexane (being commonly called as double 2,5) with cumyl peroxide (being commonly called as DCP)
Thing；
By above-mentioned mixing of rubber under 150 DEG C, 15Mpa pressure, vulcanize 14 minutes, required sample is made, to its progressive
It can test, performance test methods are identical with embodiment one, and its performance is as shown in the table.
In the above-described embodiments, reinforced filling also can be selected any in calcium carbonate, white carbon, zinc oxide, titanium dioxide
A kind of or any several combination, phosphate filler can be selected APP, red phosphorus, aluminium triphosphate, diethyl hypo-aluminum orthophosphate,
Any one in ammonium phosphate salt or any several combination, silicone oil using methyl vinyl silicon oil, high activity vinyl silicone oil,
Any one in methyl-silicone oil or any several combination, vulcanizing agent is using the double (t-butyl peroxies of 2,5- dimethyl -2,5-
Base) hexane (be commonly called as double 2,5), 2,4- dichlorides BP (being commonly called as double 2,4), in cumyl peroxide (being commonly called as DCP)
Any one or any several combination.
As seen from the above table, applied to technical solution of the present invention embodiment batten test performance layer of charcoal intensity and expansion
Multiple is greatly improved than pure silicone rubber, and the mechanical property of material also meets the mechanical property that typically requires.Namely
Say, silicon rubber composite material of the present invention also keeps its layer of charcoal intensity requirement while expansion, and mechanical property is also in silicon
It is greatly improved after the addition of oil, and meets the normal value applied usually, there is high innovative value.
The above described is only a preferred embodiment of the present invention, any formal limitation not is done to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
To any simple modification, equivalent change and modification made for any of the above embodiments, in the range of still falling within technical solution of the present invention.
Claims (10)
- A kind of 1. expandable flame retardant silicon rubber composite material, it is characterised in that：Including 100 parts of methyl vinyl silicon kautschuk, mend Strong filler 20-30 parts, expansible graphite 0-20 parts, phosphoric acid salt fire retardant 0-20 parts, vulcanizing agent 2-4 parts, silicone oil 4-6 parts, institute It is weight ratio to state material.
- 2. expandable flame retardant silicon rubber composite material according to claim 1, it is characterised in that：The reinforced filling is carbonic acid At least one of calcium, white carbon, zinc oxide, titanium dioxide.
- 3. expandable flame retardant silicon rubber composite material according to claim 1, it is characterised in that：Described phosphoric acid salt is fire-retardant Agent is at least one of APP, red phosphorus, aluminium triphosphate, diethyl hypo-aluminum orthophosphate, ammonium phosphate salt.
- 4. expandable flame retardant silicon rubber composite material according to claim 1, it is characterised in that：The silicone oil is ethylene methacrylic At least one of base silicone oil, high activity vinyl silicone oil, methyl-silicone oil.
- 5. expandable flame retardant silicon rubber composite material according to claim 1, it is characterised in that：The vulcanizing agent is 2,5- bis- At least one in methyl -2,5- bis(t-butylperoxy)s hexane, 2,4- dichlorides BP or cumyl peroxide Kind.
- 6. expandable flame retardant silicon rubber composite material according to claim 1, it is characterised in that：The expansible graphite is 10-20 parts, the phosphoric acid salt fire retardant are 10-20 parts.
- 7. a kind of preparation method of expandable flame retardant silicon rubber composite material, it is characterised in that comprise the steps：(1) by 100 parts of methyl vinyl silicon kautschuks, 20-30 parts supporting material, 0-20 parts expansible graphite, 0-20 part phosphorus Barbiturates filler is kneaded uniform；(2) it is kneaded in the mixture for obtaining 4-6 parts methyl-silicone oil addition step (1) uniform；(3) it is well mixed in the mixture for obtaining 2-4 parts vulcanizing agent addition step (2), slice obtains mixing of rubber；(4) above-mentioned mixing of rubber is vulcanized, required test piece is made.
- 8. the preparation method of expandable flame retardant silicon rubber composite material according to claim 7, it is characterised in that：The vulcanization Process is carried out under 140-170 DEG C, 10-15Mpa pressure, cure time 10-15 minutes.
- 9. the preparation method of expandable flame retardant silicon rubber composite material according to claim 7, it is characterised in that：The phosphoric acid Salt filler is through drying.
- 10. the preparation method of expandable flame retardant silicon rubber composite material according to claim 7, it is characterised in that：The step Suddenly (one) and step (2) are carried out in double roll mill or banbury.
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Cited By (5)
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| CN109266007A (en) * | 2018-09-27 | 2019-01-25 | 唐山师范学院 | Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber |
| CN110982185A (en) * | 2019-12-16 | 2020-04-10 | 应急管理部天津消防研究所 | Fireproof sealing rubber material |
| CN111647233A (en) * | 2020-07-07 | 2020-09-11 | 山东龙祥新材料科技有限公司 | Low-density foaming expansion flame-retardant ethylene propylene rubber and preparation method thereof |
| CN114716810A (en) * | 2022-04-13 | 2022-07-08 | 青岛科技大学 | Flame-retardant thermoplastic polyurethane and preparation method thereof |
| CN117567867A (en) * | 2024-01-16 | 2024-02-20 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
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| CN109266007A (en) * | 2018-09-27 | 2019-01-25 | 唐山师范学院 | Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber |
| CN110982185A (en) * | 2019-12-16 | 2020-04-10 | 应急管理部天津消防研究所 | Fireproof sealing rubber material |
| CN111647233A (en) * | 2020-07-07 | 2020-09-11 | 山东龙祥新材料科技有限公司 | Low-density foaming expansion flame-retardant ethylene propylene rubber and preparation method thereof |
| CN114716810A (en) * | 2022-04-13 | 2022-07-08 | 青岛科技大学 | Flame-retardant thermoplastic polyurethane and preparation method thereof |
| CN117567867A (en) * | 2024-01-16 | 2024-02-20 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
| CN117567867B (en) * | 2024-01-16 | 2024-04-05 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
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Application publication date: 20180406 |