CN108912604A - A kind of epoxy resin and preparation method thereof with high efficiency flame retardance - Google Patents
A kind of epoxy resin and preparation method thereof with high efficiency flame retardance Download PDFInfo
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- CN108912604A CN108912604A CN201810629897.2A CN201810629897A CN108912604A CN 108912604 A CN108912604 A CN 108912604A CN 201810629897 A CN201810629897 A CN 201810629897A CN 108912604 A CN108912604 A CN 108912604A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- 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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- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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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
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08K9/10—Encapsulated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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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
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
Abstract
The invention belongs to field of fire-proof technology, provide a kind of epoxy resin and preparation method thereof with high efficiency flame retardance.The raw material of the epoxy resin includes：Epoxy resin, fire retardant systems and curing agent；Fire retardant systems include fire retardant and synergist.The epoxy resin with high efficiency flame retardance has excellent flame retardant property, while being able to maintain the physical mechanical property of its script.The preparation method includes mixing epoxy resin and fire retardant systems, vacuumizes to obtain the first mixture；It is added into the first mixture by curing agent, then vacuumizes to obtain the second mixture；Second mixture is added in mold, is vacuumized；Then it deflates, then solidifies, then heat up resolidification, then elevated cure, cooling.The preparation method design science, preparation process environmental protection, is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to field of fire-proof technology, specifically, be related to a kind of epoxy resin with high efficiency flame retardance and
Preparation method.
Background technique
It is found by researches that epoxy resin is widely noticed due to its excellent performance.But because itself flame retardant property is poor
The reason of, for the limit oxygen index of epoxy resin 19.8% or so, this condition limits the application of epoxy resin.The prior art
In, being modified in a manner of improving its flame retardant property to epoxy resin has very much, however most when its flame retardant property mentions
The performances such as its mechanics can be destroyed simultaneously while high, and the requirement of script is not achieved, still will limit the application of epoxy resin.
Summary of the invention
For deficiency above-mentioned in the prior art, the first object of the present invention is to provide a kind of with high efficiency flame retardance
Epoxy resin；The epoxy resin with high efficiency flame retardance has excellent flame retardant property, while being able to maintain its script
Physical mechanical property.
For deficiency above-mentioned in the prior art, the second object of the present invention is to provide a kind of with high efficiency flame retardance
Epoxy resin preparation method；The preparation method design science, preparation process environmental protection, is suitable for large-scale industrial production.
In order to achieve the above object, the solution that the present invention uses is：
A kind of epoxy resin with high efficiency flame retardance, raw material in parts by weight, including：Epoxy resin 73-
78 parts, 12-22 parts of fire retardant systems and 10 parts of curing agent；According to parts by weight, fire retardant systems include 10-20 parts of fire retardant
With 2 parts of synergist.
A kind of preparation method of the above-mentioned epoxy resin with high efficiency flame retardance, including by epoxy resin and fire retardant body
System's mixing, vacuumizes 18-22min under the conditions of vacuum degree is 0.06Mpa, obtains the first mixture；Add into the first mixture
Enter curing agent, then vacuumize 2-3min under the conditions of vacuum degree is in 0.06MPa, obtains the second mixture；By the second mixing
Object is added in mold, vacuumizes 5-6min under the conditions of vacuum degree is greater than 0.07Mpa；Then deflation 4- is carried out under the conditions of 80 DEG C
5 times, then solidify 2h, be then warming up to 100 DEG C of solidification 2h, then after being warming up to 120 DEG C of solidification 3h, it is cooling.
A kind of beneficial effect of epoxy resin with high efficiency flame retardance provided by the invention and preparation method thereof is：
(1) epoxy resin provided by the invention with high efficiency flame retardance, using epoxy resin, fire retardant systems and
Curing agent is compounded, and a kind of epoxy resin with high efficiency flame retardance is creatively had developed.This has highly effective flame-retardant
The epoxy resin of performance has excellent flame retardant property, while being able to maintain the physical mechanical property of its script.The present invention takes
Epoxy resin, fire retardant systems and curing agent are compounded according to above-mentioned parts by weight, between each component can coordinated,
So that the flame retardant property of product obtained is more excellent, the physical mechanical property of script will not be excessively destroyed.
(2) present invention provides, and there is the preparation method design science of the epoxy resin of high efficiency flame retardance to be simple and efficient, respectively
Coordinated between reaction condition, environmental protection, flame retardant property and excellent in mechanical performance can be prepared has highly effective flame-retardant
The epoxy resin of energy.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to a kind of epoxy resin with high efficiency flame retardance provided in an embodiment of the present invention and preparation method thereof into
Row illustrates.
A kind of epoxy resin with high efficiency flame retardance, raw material in parts by weight, including：Epoxy resin 73-
78 parts, 12-22 parts of fire retardant systems and 10 parts of curing agent.
The selection of above-mentioned each raw material and proportion pass through scientific design, so that association can be played by cooperating between various raw materials
With the effect of synergy, using this proportion, can be greatly improved in the case where not destroying the mechanical property of epoxy resin final
The flame retardant property of product.
It should be noted that in the present embodiment, according to parts by weight, fire retardant systems include 10-20 parts of fire retardant and
2 parts of synergist.
Wherein, the classification of fire retardant is not particularly limited, and further, fire retardant includes 6-12 parts of ammonium polyphosphate, trimerization
2-4 parts and pentaerythrite 2-4 parts of cyanamide.Inventor creatively has found, constitutes one using the fire retardant that above-mentioned raw materials form
The fire-retardant medium of kind " green " can replace the halogen-containing fire retardant for destroying atmosphere, meet the environmental requirement of the world today.
Wherein, the classification of synergist is not particularly limited, and further, synergist includes inflatable type graphite, methyl phosphorus
One of dimethyl phthalate or modified red phosphorus.Those synergists are by promoting into charcoal or changing the principles such as Char Residues Structure, to improve
Flame retardant effect.
It is compounded according to above-mentioned fire retardant and synergist, inventor creatively has found to constitute a kind of compound, should
Compound is non-volatile in burning, will not generate corrosive gas, very environmental protection.
It should be noted that the modification red phosphorus in the present embodiment is further preferably melamine formaldehyde resin encapsulated red phosphorus.
Melamine formaldehyde resin encapsulated red phosphorus is reduced compared to common red phosphorus, the water imbibition of red phosphorus and the burst size of hydrogen phosphide.
It should be noted that in the present embodiment, the selection of curing agent is not specifically limited, further, inventor is adopted
Find that it has the temperature deformed compared with high heat resistance with m-phenylene diamine (MPD), dielectricity relatively strong with respect to the material mechanical performance of other materials
Energy and corrosion resistance are all very good.
A kind of preparation method of the epoxy resin with high efficiency flame retardance, including：Epoxy resin is pre-processed：?
Before mixing, epoxy resin is weighed after 80 DEG C of baking 25-35min, in favor of increasing the mobility of epoxy resin convenient for subsequent
Experiment carries out.Then it is vacuumized under the conditions of vacuum degree is 0.06MPa, to reduce the bubble in epoxy resin.It needs to illustrate
Be, epoxy resin vacuumize during include：Every 3-5min that crosses stirs epoxy resin taking-up, will be in underlying epoxy
It is vacuumized again after bubble agitation to surface；It repeats 2-3 times, continues 20-25min, to accelerate the removing of bubble.
Then, fire retardant systems are pre-processed：Before mixing, fire retardant systems are subjected to preliminary drying 10min, to remove
The moisture that may be had in flame-retardant system.
Then, epoxy resin and fire retardant systems being mixed, stirring makes fire retardant systems be uniformly dispersed in the epoxy,
18-22min is vacuumized under the conditions of vacuum degree is 0.06Mpa again, in favor of removing bubble, obtains the first mixture.Then, to
It is added in first mixture by curing agent, then vacuumizes 2-3min under the conditions of vacuum degree is in 0.06MPa, in favor of removing degassing
Bubble, obtains the second mixture.Then the temperature of vulcanizing press is risen to 80 DEG C, then mold is added on vulcanizing press
Heat treatment smears one layer of dimethicone on mold and is used as release agent.Then the second mixture is poured into mould while stirring again
In tool, 5-6min is vacuumized under the conditions of vacuum degree is greater than 0.07Mpa.And observe the variation feelings of the second mixture in mold
Condition can generate a large amount of bubble in this course, and bubble will be reduced significantly as time increases, finally observe second
Whether the bubble in mixture completely disappears.Then it is carried out under the conditions of 80 DEG C deflation 4-5 times, then solidifies 2h, then heat up
To 100 DEG C of solidification 2h, then after being warming up to 120 DEG C of solidification 3h.Subsequent natural cooling, with the residual temperature using vulcanizing press to wherein
Carrying out effect there are no the key of crosslinking keeps its fully crosslinked.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 12 parts of 78 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
6 parts of ammonium, 2 parts of melamine, 2 parts of pentaerythrite, inflatable 2 parts of type graphite).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 25min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 2 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 18min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 2min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 5min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 4 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 2
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 17 parts of 73 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
9 parts of ammonium, 3 parts of melamine, 3 parts of pentaerythrite, inflatable 2 parts of type graphite).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 25min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 3 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 18min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 2min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 5min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 4 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 3
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 22 parts of 68 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
12 parts of ammonium, 4 parts of melamine, 4 parts of pentaerythrite, inflatable 2 parts of type graphite).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 25min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 3 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 18min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 2min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 5min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 4 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 5
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 17 parts of 73 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
9 parts of ammonium, 3 parts of melamine, 3 parts of pentaerythrite, modified 2 parts of red phosphorus).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 35min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 5min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 3 times, continues 25min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 22min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 3min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 6min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 5 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 6
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 15 parts of 75 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
7.5 parts of ammonium, 3.75 parts of melamine, 3.75 parts of pentaerythrite, inflatable 2 parts of type graphite).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 30min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 4min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 3 times, continues 22min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 20min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 3min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 6min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 5 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 7
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 15 parts of 75 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
7.5 parts of ammonium, 3.75 parts of melamine, 3.75 parts of pentaerythrite, 2 parts of methyl-phosphoric acid dimethyl ester).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 30min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 4min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It repeats 2-3 times, continues 22min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 20min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 3min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 6min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 5 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Embodiment 8
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 15 parts of 75 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
7.5 parts of ammonium, 3.75 parts of melamine, 3.75 parts of pentaerythrite, modified 2 parts of red phosphorus).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 30min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 4min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；Repeat secondary, lasting 22min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 20min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 3min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 6min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 5 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Comparative example 1
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 23 parts of 67 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
13 parts of ammonium, 5 parts of melamine, 5 parts of pentaerythrite, modified 2 parts of red phosphorus).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 25min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 2 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 18min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 2min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 5min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 4 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Comparative example 2
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 8 parts of 82 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
4 parts of ammonium, 1 part of melamine, 1 part of pentaerythrite, modified 2 parts of red phosphorus).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 80 DEG C of baking 25min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 2 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 18min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 2min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 5min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 4 times under the conditions of 80 DEG C, then solidifies 2h, be then warming up to 100 DEG C of solidification 2h, then be warming up to 120 DEG C of solidification 3h
Afterwards, cooling.
Comparative example 3
A kind of epoxy resin with high efficiency flame retardance is present embodiments provided,
It prepares raw material：Score meter by weight, 15 parts of 75 parts of epoxy resin, 10 parts of meta-xylene, flame-retardant system (polyphosphoric acids
7.5 parts of ammonium, 3.75 parts of melamine, 3.75 parts of pentaerythrite, modified 2 parts of red phosphorus).
Preparation method：
The pretreatment of epoxy resin：Before mixing, epoxy resin is weighed after 75 DEG C of baking 30min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa；Epoxy resin includes during vacuumizing：Every 3min that crosses stirs epoxy resin taking-up,
It will be vacuumized again after bubble agitation to surface in underlying epoxy；It is repeated 3 times, continues 20min；
The pretreatment of fire retardant systems：Before mixing, fire retardant systems are subjected to preliminary drying 10min；
Epoxy resin and fire retardant systems are mixed, vacuumize 15min under the conditions of vacuum degree is 0.06Mpa, obtain the
One mixture；It is added into the first mixture by curing agent, then vacuumizes 1min under the conditions of vacuum degree is in 0.06MPa, obtain
To the second mixture；Second mixture is added in mold, vacuumizes 4min under the conditions of vacuum degree is greater than 0.07Mpa；Then
It carries out deflating 3 times under the conditions of 75 DEG C, then solidifies 2h, be then warming up to 90 DEG C of solidification 2h, then be warming up to 110 DEG C of solidification 3h
Afterwards, cooling.
Experimental example 1：Impact property test
Experimental method：By pure epoxy resin, the product that embodiment 1-8 and comparative example 1-3 are provided is set as experimental group 1-
12；Using the impact strength of the shock machine difference test experiments group 1-12 of model XJJD-5.Specimen size is 80*10*
3.2mm3, non-notch test, test result is as shown in table 1：
1 unnotched impact strength test result of table
| Group number | 1 | 2 | 3 | 4 | 5 | 6 |
| Impact strength (KJ/m2) | 0.0197 | 0.0189 | 0.0174 | 0.0128 | 0.0165 | 0.0137 |
| Group number | 7 | 8 | 9 | 10 | 11 | 12 |
| Impact strength (KJ/m2) | 0.0174 | 0.0117 | 0.0091 | 0.0021 | 0.0023 | 0.0032 |
From the data in table 1, it can be seen that product is made within the scope of each raw material proportioning provided in an embodiment of the present invention, and using this
Product obtained within the scope of parameters involved in the preparation method that inventive embodiments provide, impact strength are better than not
Using product obtained in above range provided in an embodiment of the present invention.
Embodiment 2：Limit oxygen index test
Experimental method：By pure epoxy resin, the product that embodiment 1-8 and comparative example 1-3 are provided is set as experimental group 1-
12；Using the limit oxygen index value of HC-2C type oxygen index instrument test experiments group 1-12, the size of sample is 130*13*3.2mm3,
Test result is as shown in table 1：
2 limit oxygen index test result of table
| Group number | 1 | 2 | 3 | 4 | 5 | 6 |
| Limit oxygen index LOI (%) | 22 | 26.5 | 30 | 32 | 29 | 30 |
| Group number | 7 | 8 | 9 | 10 | 11 | 12 |
| Limit oxygen index LOI (%) | 29 | 29 | 28.5 | 22 | 23 | 24 |
From the data in table 2, it can be seen that the LOI value of pure epoxy resin is 22, and while burning in air can also generate it is a large amount of black
Cigarette.Product is made within the scope of each raw material proportioning provided in an embodiment of the present invention, and uses system provided in an embodiment of the present invention
Product (experimental group 2-9) obtained, flame retardant property are greatly improved within the scope of parameters involved in Preparation Method.And it is real
The flame retardant property of the product of group 2-9 is tested better than not using product (experiment obtained in above range provided in an embodiment of the present invention
Group 10-12), illustrate that product is made within the scope of each raw material proportioning provided in an embodiment of the present invention and the embodiment of the present invention mentions
Product obtained has more excellent flame retardant property within the scope of parameters involved in the preparation method of confession.
Embodiment 3：Contact angle test
Experimental method：By pure epoxy resin, the product that embodiment 1-8 and comparative example 1-3 are provided is set as experimental group 1-
12；The product contact angle test to water that carries out experimental group 1-12 is surveyed on instrument (Dataphysics) using JCY collection of contact angle,
It is tested at room temperature, test result is as shown in table 3：
The test of 3 water contact angle of table
| Group number | 1 | 2 | 3 | 4 | 5 | 6 |
| Water contact angle (°) | 56.740 | 76.000 | 69.280 | 74.780 | 73.735 | 84.405 |
| Group number | 7 | 8 | 9 | 10 | 11 | 12 |
| Water contact angle (°) | 72.860 | 72.050 | 80.325 |
0 ° of 90 ° of < water contact angle <, fluid wetable solid, and it is smaller, wetability is better, cries hydrophilic contact angle.90 ° of <
180 ° of water contact angle <, the nonwetting solid of liquid is also hydrophobic contact angle or hydrophobic contact angle.From the data in table 3, it can be seen that this
The hydrophobicity for testing the pure epoxy resin substrate of test is poor (56.74 ° of water contact angle), and the hydrophobic performance of experimental group 2-9 becomes
Good (water contact angle increases, maximum up to 84.405 °), this is because produced after flame-retardant system is added in epoxy resin it is special
Structure or phosphorus-nitrogen system fire retardant and water compatibility it is bad caused by.And the increasing of the hydrophobic performance of experimental group 10-12
Add not as good as experimental group 2-9, illustrates that product is made within the scope of each raw material proportioning provided in an embodiment of the present invention and the present invention is real
Applying involved in the preparation method of example offer product obtained within the scope of parameters has more excellent hydrophobic performance.
In conclusion using a kind of epoxy resin with high efficiency flame retardance provided by the invention；This has efficient resistance
The epoxy resin for firing performance has excellent flame retardant property, while being able to maintain the physical mechanical property of its script.Using this hair
A kind of preparation method of epoxy resin with high efficiency flame retardance of bright offer；The preparation method design science, prepared
Cheng Huanbao is suitable for large-scale industrial production.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of epoxy resin with high efficiency flame retardance, it is characterised in that：Its raw material in parts by weight, including：Ring
73-78 parts of oxygen resin, 12-22 parts of fire retardant systems and 10 parts of curing agent；According to parts by weight, the fire retardant systems include
10-20 parts and 2 parts of synergist of fire retardant.
2. the epoxy resin according to claim 1 with high efficiency flame retardance, it is characterised in that：Score meter by weight,
The fire retardant includes 6-12 parts of ammonium polyphosphate, 2-4 parts of melamine and 2-4 parts of pentaerythrite.
3. the epoxy resin according to claim 1 with high efficiency flame retardance, it is characterised in that：Score meter by weight,
The synergist includes one of inflatable type graphite, methyl-phosphoric acid dimethyl ester or modified red phosphorus.
4. the epoxy resin according to claim 3 with high efficiency flame retardance, it is characterised in that：The modified red phosphorus is
Melamine formaldehyde resin encapsulated red phosphorus.
5. the epoxy resin according to claim 1 with high efficiency flame retardance, it is characterised in that：The curing agent includes
Meta-xylene.
6. a kind of preparation method of the epoxy resin according to claim 1 with high efficiency flame retardance, which is characterized in that
Including：The epoxy resin and the fire retardant systems are mixed, vacuumize 18- under the conditions of vacuum degree is 0.06Mpa
22min obtains the first mixture；It is added into first mixture by the curing agent, then in vacuum degree in 0.06MPa
Under the conditions of vacuumize 2-3min, obtain the second mixture；Second mixture is added in mold, is greater than in vacuum degree
5-6min is vacuumized under the conditions of 0.07Mpa；Then it is carried out under the conditions of 80 DEG C deflation 4-5 times, then solidifies 2h, be then warming up to
100 DEG C of solidification 2h, then after being warming up to 120 DEG C of solidification 3h, it is cooling.
7. the preparation method of the epoxy resin according to claim 6 with high efficiency flame retardance, it is characterised in that：Also wrap
Include the pretreatment of epoxy resin：Before mixing, the epoxy resin is weighed after 80 DEG C of baking 25-35min, then in vacuum degree
To be vacuumized under the conditions of 0.06MPa.
8. the preparation method of the epoxy resin according to claim 7 with high efficiency flame retardance, it is characterised in that：It is described
Epoxy resin includes during vacuumizing：Every 3-5min that crosses stirs epoxy resin taking-up, by asphalt mixtures modified by epoxy resin described in lower layer
It is vacuumized again after bubble agitation to surface in rouge；It repeats 2-3 times, continues 20-25min.
9. the preparation method of the epoxy resin according to claim 6 with high efficiency flame retardance, it is characterised in that：Also wrap
Include the pretreatment of fire retardant systems：Before mixing, the fire retardant systems are subjected to preliminary drying 10min.
10. the preparation method of the epoxy resin according to claim 6 with high efficiency flame retardance, it is characterised in that：Institute
Mold is stated before use, further including preheating after first smearing one layer of dimethicone.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114316550A (en) * | 2022-01-29 | 2022-04-12 | 清华大学 | Resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100048766A1 (en) * | 2006-02-23 | 2010-02-25 | Yu Hsain Cheng | Halogen-free phosphorous epoxy resin composition |
| CN103539965A (en) * | 2013-10-19 | 2014-01-29 | 山东吉青化工有限公司 | Efficient environment-friendly flame retardant |
| CN106380788A (en) * | 2016-10-24 | 2017-02-08 | 西华大学 | Halogen-free flame retardant, halogen-free flame-retarding epoxy resin and preparation method thereof |
-
2018
- 2018-06-19 CN CN201810629897.2A patent/CN108912604A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100048766A1 (en) * | 2006-02-23 | 2010-02-25 | Yu Hsain Cheng | Halogen-free phosphorous epoxy resin composition |
| CN103539965A (en) * | 2013-10-19 | 2014-01-29 | 山东吉青化工有限公司 | Efficient environment-friendly flame retardant |
| CN106380788A (en) * | 2016-10-24 | 2017-02-08 | 西华大学 | Halogen-free flame retardant, halogen-free flame-retarding epoxy resin and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316550A (en) * | 2022-01-29 | 2022-04-12 | 清华大学 | Resin and preparation method thereof |
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