CN106633917B - A kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and preparation method thereof - Google Patents
A kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/14—Peroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/527—Cyclic esters
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
- C08K5/5333—Esters of phosphonic acids
- C08K5/5357—Esters of phosphonic acids cyclic
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/328—Phosphates of heavy metals
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and preparation method thereof.The material consists of the following components in percentage by weight: silicon rubber 68.0%-82.0%, nano-meter flame retardants 0.5%-5.0%, nitrogen phosphorus system expanding fire retardant 18.0%-25.0%, vulcanizing agent 0.5%-2.5%.Rubber material of the invention is halogen-free and other harmful substances, toxic gas will not be generated in combustion process causes secondary pollution, nano-meter flame retardants are uniformly dispersed in silicone rubber matrix, only need the combustibility that just can significantly reduce silicon rubber on a small quantity, and the mechanical performance of silicon rubber can also be made to improve, nitrogen phosphorus flame retardant can assign silicon rubber excellent flame retardant property, and the fire retardant mechanism of the two is that condensed phase is fire-retardant, synergy is significant, when the two is used in compounding, the flame retardant property of silicon rubber can be improved, the mechanical performance of silicon rubber can be made to be maximally maintained again.
Description
Technical field
The present invention relates to polymer composites to be blended, material flame retardant area, and in particular to a kind of nano-meter flame retardants and nitrogen
Phosphorus system expanding fire retardant cooperative flame retardant silastic material and preparation method thereof.
Background technique
Since the commercialization of the silicon rubber forties in last century, various silicone rubber products emerge one after another, and silicon rubber has excellent
Different biocompatibility, resistant to chemical etching, electrical insulating property etc. are widely used in the neck such as health care, communications and transportation, electronic apparatus
Domain.But silicon rubber easily burns, and one it is ignited will release a large amount of heat, seriously limit silicon rubber apply model
It encloses.Therefore the flame-retardant modified of silicon rubber is particularly important.
Currently, halogen flame influences the advantages that small because of its flame retarding efficiency height, on the mechanical performance of material, market is occupied
Half of the country, but the material handled through halogen flame can discharge toxic when burning, and be corrosive gas and big
The smog of amount and cause secondary pollution, therefore, both at home and abroad to limitation, the cry for being forbidden to use halogen flame is higher and higher.And
The characteristics of expanding fire retardant is due to its Halogen, low cigarette, low toxicity, non-corrosive gas, concern universal by people in recent years.Add
One layer of fluffy carbonaceous froth bed for having hole enclosed construction can be formed on surface when the polymer combustion of expansion type flame retardant by having added.One
Denier is formed, itself is non-ignitable, but can weaken the heat transfer between polymer and heat source, and prevent gas diffusion.Once burning not
Polymer to enough fuel and oxygen, burning will self-extinguishment.This porous layer of charcoal has heat-insulated, oxygen barrier, without dripping off simultaneously
Make the effect of flame self-extinguishment.Therefore, expandable flame retardant technology has become very active one of fire-retardant research field, but expands resistance
Agent and matrix poor compatibility are fired, is affected to the mechanical property of materials, causes to be difficult to apply in engineering.With the hair of nanotechnology
Exhibition, nano flame retardant technology have become an important research hot spot of flame retardant area.Only need to add receiving for minute quantity (less than 5%)
Rice fire retardant, can significantly reduce the combustibility of material, and the addition of nano-meter flame retardants can also make the mechanical performance of material
It improves.Nano-meter flame retardants are introduced to the nitrogen phosphorus Intumescent Retardant System of environmental protection, constitute nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant
Cooperative flame retardant silicon rubber, the characteristics of both nano-meter flame retardants and nitrogen phosphorus expanding fire retardant can be taken into account；Silicon rubber can be improved
Flame retardant property, and the mechanical performance of silicon rubber can be made to be maximally maintained.
Therefore, the invention discloses a kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and
Preparation method.There is the silastic material prepared according to the method good flame retardant property to be able to maintain higher machinery again
Performance.Currently, there are no the reports of this kind of silastic material in silicon rubber flame-retardant field.
Summary of the invention
It is an object of the invention to overcome expanding fire retardant to deteriorate matrix mechanical performance, a kind of nano flame retardant is provided
Agent and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and preparation method thereof, the anti-flammability that material of the invention has had both
Energy and mechanical performance.
What the purpose of the present invention was achieved through the following technical solutions.
A kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material, the material is by following weight hundred
The group of ratio is divided to be grouped as: silicon rubber 68.0%-82.0%, nano-meter flame retardants 0.5%-5.0%, nitrogen phosphorus system expanding fire retardant
18.0%-25.0%, vulcanizing agent 0.5%-2.5%.
Preferably, the silicon rubber is dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicon rubber
One or more of glue, fluorine silicone rubber, nitrile silicone rubber and diethyl silicon rubber.
Preferably, the nano-meter flame retardants be galapectite, hydrotalcite, montmorillonite, layered double-hydroxide, basic zirconium phosphate,
One or more of graphite oxide and carbon nanotube.
Preferably, nitrogen phosphorus system's expanding fire retardant is 2,4,8,10- tetra- oxygen -3,9 hosphospiro [5,5] hendecanes -
3.9 dioxy -3,9-, bis- melamine salt, three (neopentyl glycol phosphate-phosphorus-methylene) amine, neopentyl glycol phosphate melamine
At least one of ammonium salt and polyphosphoric acid amine.
Preferably, the vulcanizing agent is 2,4- dichlorobenzoperoxide, bis- (the tert-butyl mistakes of 2,5- dimethyl -2,5-
One or more of oxygroup) hexane, benzoyl peroxide and the different phenylpropyl alcohol of peroxidating two.
The preparation side of a kind of above-described nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material
Method, method includes the following steps:
By silicon rubber, nano-meter flame retardants, nitrogen phosphorus system's expanding fire retardant and vulcanizing agent in open mill or mixing at 15-40 DEG C
It is kneaded 15-20min in machine, then carries out compression molding 10-20min at 100-140 DEG C with compression molding instrument and obtains nanometer resistance
Fire agent and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.
Compared with prior art, the invention has the advantages that and technical effect:
(1) nano-meter flame retardants of the invention and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material be halogen-free and
Other harmful substances will not generate toxic gas in combustion process and cause secondary pollution；
(2) nano-meter flame retardants of the invention and nano-meter flame retardants in nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material
It is uniformly dispersed in silicone rubber matrix, only needs the combustibility that just can significantly reduce silicon rubber on a small quantity, and silicon rubber can also be made
Mechanical performance improves；
(3) fire retardant mechanism of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant is that same position condensed phase is fire-retardant, and the two has
The fire-retardant range of silicon rubber and non halogen has not only been widened in the utilization of good synergistic effects, nano-meter flame retardants, is also the expansion of nitrogen phosphorus system
Fire retardant provides a kind of good fire retarding synergist.
Detailed description of the invention
Fig. 1 is the SEM spectrogram that montmorillonite disperses in silicone rubber matrix in embodiment 1.
Fig. 2 is the SEM spectrogram that basic zirconium phosphate disperses in silicone rubber matrix in embodiment 2.
Fig. 3 is the SEM spectrogram that wollastonite disperses in silicone rubber matrix in embodiment 3.
Fig. 4 is the SEM spectrogram that galapectite disperses in silicone rubber matrix in embodiment 4.
Specific embodiment
In order to preferably describe and understand the present invention, below with reference to embodiment and attached drawing to specific implementation of the invention make into
One step explanation, but the scope of protection of present invention is not limited to the scope of the embodiments.
Embodiment 1
By 68g methyl phenyl vinyl silicone rubber, 5g montmorillonite, 18g tri- (neopentyl glycol phosphate-phosphorus-methylene) amine,
0.5g 2,4- dichlorobenzoperoxide are kneaded 15min at 15 DEG C in open mill, then with compression molding instrument in 100 DEG C
Lower progress compression molding 10min obtains nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.Fig. 1 is to cover
The SEM spectrogram that de- soil disperses in silicone rubber matrix.From Fig. 1 it can be found that montmorillonite disperses very well in silicone rubber matrix.
The mechanical property of nano-meter flame retardants manufactured in the present embodiment and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material and fire-retardant
Performance is shown in Table 1.
Embodiment 2
By 82g methyl vinyl silicone rubber, 0.5g basic zirconium phosphate, 25g polyphosphoric acid amine, 2.5g 2,4- dichloro benzoyl peroxide first
Acyl is kneaded 20min at 25 DEG C in open mill, then carries out compression molding 14min at 110 DEG C with compression molding instrument and obtains
Nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.Fig. 2 is that basic zirconium phosphate disperses in silicone rubber matrix
SEM spectrogram.From Fig. 2 it can be found that basic zirconium phosphate is evenly dispersed in silicone rubber matrix.Nano-meter flame retardants manufactured in the present embodiment
1 is shown in Table with the mechanical property and flame retardant property of nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.
Embodiment 3
By 75g dimethyl silicone rubber, 2.5g wollastonite, 22g neopentyl glycol phosphate melamine salt, 2g 2,5- diformazan
Base -2,5- bis(t-butylperoxy) is kneaded 18min at 35 DEG C in open mill, then with compression molding instrument at 125 DEG C
It carries out compression molding 17min and obtains nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.Fig. 3 is silicon ash
The SEM spectrogram that stone disperses in silicone rubber matrix.From Fig. 3 it can be found that wollastonite disperses very well in silicone rubber matrix.This reality
Apply the nano-meter flame retardants of example preparation and the mechanical property and flame retardant property of nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material
It is shown in Table 1.
Embodiment 4
By 78.5g dimethyl silicone rubber, 3g galapectite, 19g polyphosphoric acid amine, the bis- (tert-butyls of 1g 2,5- dimethyl -2,5-
Peroxy) 18min is kneaded in open mill at 40 DEG C, compression molding 20min is then carried out at 140 DEG C with compression molding instrument
Obtain nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.Fig. 4 is galapectite in silicone rubber matrix
The SEM spectrogram of dispersion.From Fig. 4 it can be found that galapectite disperses very well in silicone rubber matrix, soilless sticking.The present embodiment preparation
Nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material mechanical property and flame retardant property be shown in Table 1.
Table 1
As shown in Table 1, nano-meter flame retardants of the invention have with nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material
Good flame retardant property is able to maintain higher mechanical performance again.
Claims (4)
1. a kind of nano-meter flame retardants and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material, which is characterized in that the material by
Following components in percentage by weight composition: silicon rubber 68.0%-82.0%, nano-meter flame retardants 0.5%-5.0%, nitrogen phosphorus system expandable flame retardant
Agent 18.0%-25.0%, vulcanizing agent 0.5%-2.5%；
The nano-meter flame retardants are galapectite, hydrotalcite, montmorillonite, layered double-hydroxide, basic zirconium phosphate, graphite oxide and carbon
One or more of nanotube；
Nitrogen phosphorus system's expanding fire retardant is -3.9 dioxy -3,9- of 2,4,8,10- tetra- oxygen -3,9 hosphospiro [5,5] hendecane
Two melamine salts, three (neopentyl glycol phosphate-phosphorus-methylene) amine, neopentyl glycol phosphate melamine salt and polyphosphoric acids
At least one of amine.
2. a kind of nano-meter flame retardants according to claim 1 and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material,
It is characterized in that, the silicon rubber be dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber,
One or more of fluorine silicone rubber, nitrile silicone rubber and diethyl silicon rubber.
3. a kind of nano-meter flame retardants according to claim 1 and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material,
It is characterized in that, the vulcanizing agent is 2,4- dichlorobenzoperoxide, 2,5- dimethyl -2,5- bis(t-butylperoxy)
One or more of hexane, benzoyl peroxide and the different phenylpropyl alcohol of peroxidating two.
4. a kind of described in any item nano-meter flame retardants of claim 1-3 and nitrogen phosphorus system expanding fire retardant cooperative flame retardant silicon rubber material
The preparation method of material, which comprises the following steps:
By silicon rubber, nano-meter flame retardants, nitrogen phosphorus system's expanding fire retardant and vulcanizing agent at 15-40 DEG C in open mill or mixer
It is kneaded 15-20min, then compression molding 10-20min is carried out at 100-140 DEG C with compression molding instrument and obtains nano-meter flame retardants
With nitrogen phosphorus system expanding fire retardant cooperative flame retardant silastic material.
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| CN107236305A (en) * | 2017-07-07 | 2017-10-10 | 东莞市联洲知识产权运营管理有限公司 | A kind of fire-resisting cable silicon rubber composite material and preparation method thereof |
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| CN109705766A (en) * | 2018-12-24 | 2019-05-03 | 昆山诺泰普复合新材料有限公司 | A kind of high-performance refractory type silicon rubber self-adhesive tape and its preparation process |
| CN112662184B (en) * | 2020-12-08 | 2022-10-28 | 清远市普塞呋磷化学有限公司 | Flame-retardant silicone rubber material and preparation method thereof |
| CN112812572B (en) * | 2021-01-26 | 2022-10-04 | 国光电器股份有限公司 | Silicone rubber and preparation method and application thereof |
| CN113881149A (en) * | 2021-09-24 | 2022-01-04 | 安徽京鸿密封件技术有限公司 | Low-hardness V0-grade flame-retardant ethylene propylene rubber material |
| CN114031812A (en) * | 2021-11-23 | 2022-02-11 | 上海聚千新材料发展有限公司 | Nitrogen-phosphorus flame retardant and preparation method thereof |
| CN114181536B (en) * | 2021-12-24 | 2023-05-09 | 清远市普塞呋磷化学有限公司 | Flame-retardant silicone rubber material and preparation method and application thereof |
| CN115322572B (en) * | 2022-08-11 | 2023-06-13 | 深圳市泰科科技有限公司 | Flame-retardant fireproof silicone rubber material for cables and preparation method thereof |
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