CN108084660B - A kind of expansion type fire retarding epoxide resin and preparation method thereof - Google Patents
A kind of expansion type fire retarding epoxide resin and preparation method thereof Download PDFInfo
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- CN108084660B CN108084660B CN201711439481.6A CN201711439481A CN108084660B CN 108084660 B CN108084660 B CN 108084660B CN 201711439481 A CN201711439481 A CN 201711439481A CN 108084660 B CN108084660 B CN 108084660B
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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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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
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Abstract
The present invention relates to a kind of expansion type fire retarding epoxide resin, component and each component mass percent are as follows: epoxy resin 42.5%~85%；Curing agent 5%~42.5%；Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；The ratio between mass fraction of ammonium polyphosphate and calcium gluconate is 4:1~10:1 in the ammonium polyphosphate and gluconic acid calcium complexes；The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%~35.5%, UL-94 vertical combustion rank is V-1~V-0 grades.The invention also discloses preparation methods.Present invention employs ammonium polyphosphate and gluconic acid calcium complexes as expansion type flame retardant fire retarding epoxide resin, and fire retardant additive amount is low, and flame retarding efficiency is high, with excellent flame retardant property, used ammonium polyphosphate and calcium gluconate price are low, convenient sources, convenient for promoting the use of.
Description
Technical field
The present invention relates to Halogenless fire retarded epoxy resin technical field more particularly to a kind of expansion type fire retarding epoxide resin and its
Preparation method.
Background technique
Epoxy resin cured product is due to having many advantages, such as that mechanical strength height, insulating properties, thermal stability be good, chemical corrosion resistance
It is widely used in the fields such as the insulating materials of coating, adhesive, fibre reinforced composites, electronic and electrical equipment.However, ring
Oxygen resin is a kind of combustible material, and can generate a large amount of dense smokes and toxic and harmful gas after burning, and is not able to satisfy and wants to fire-retardant
Higher application field is sought, thus significantly limits the application of epoxy resin.
Expandable flame retardant is current halogen-free flameproof priority fields of study, because it has the characteristics that Halogen, low cigarette, low toxicity, quilt
It is widely used in flame-retardant polymer.The patent report of Publication No. CN105037689A fatty amine ammonium polyphosphate modifying is applied to
Excellent flame retardant effect is obtained in epoxy resin, however the ammonium polyphosphate modifying is used as reactive flame retardant, preparation
The process is more complicated, and process is relatively complicated.Document (RSC Adv.2017,7, pp 35619-35628) reports ammonium polyphosphate association
With the work of cuprous oxide fire retarding epoxide resin.The result shows that individually adding 21% ammonium polyphosphate, the vertical combustion of epoxy resin
Rank is stepless；After ammonium polyphosphate is compounded with cuprous oxide, although vertical combustion rank is improved to V-0 grades, additive amount is still
More a height of 17%.
Calcium gluconate shows the ability of excellent generation intumescent carbon-coating in combustion, however it is fire-retardant
Application on field is never reported.Thus it is contemplated that it is compounded with ammonium polyphosphate, ammonium polyphosphate is improved in the epoxy
Flame retarding efficiency, reduce the additive amount of fire retardant, to reduce cost.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of intumescent resistance with excellent fire-retardancy
Fire epoxy resin and preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of expansion type fire retarding epoxide resin, component and each component mass percent are as follows:
Epoxy resin 42.5%~85%；
Curing agent 5%~42.5%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%~35.5%, UL-94 vertical combustion rank is V-1
~V-0 grades.
Preferably, a kind of expansion type fire retarding epoxide resin, component and each component mass percent are as follows:
Epoxy resin 65%~75%；
Curing agent 15%~20%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin be 30.9%~35%, UL-94 vertical combustion rank be V-1~
V-0 grades.
The epoxy resin is E44 epoxy resin or E51 epoxy resin.
The curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and low molecular polyamides tree
Any one of rouge 650.
The ratio between ammonium polyphosphate and the mass fraction of calcium gluconate are in the ammonium polyphosphate and gluconic acid calcium complexes
4:1~10:1.
Preferably, ammonium polyphosphate and the quality of calcium gluconate point in the ammonium polyphosphate and gluconic acid calcium complexes
The ratio between number is 6:1~8:1.
Preferably, the expansion type fire retarding epoxide resin with a thickness of 3.2mm.
A kind of preparation method of expansion type fire retarding epoxide resin, the preparation method comprises the following steps:
1) epoxy resin, curing agent, ammonium polyphosphate and gluconic acid calcium complexes are weighed by each component mass percent；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The invention adopts the above technical scheme, uses ammonium polyphosphate and gluconic acid calcium complexes as expansion type flame-retarding
Agent fire retarding epoxide resin, fire retardant additive amount is low, and flame retarding efficiency is high, has excellent flame retardant property, used ammonium polyphosphate
It is low with calcium gluconate price, convenient sources, convenient for promoting the use of.Compared with prior art, it has the advantage that
(1) expansion type fire retarding epoxide resin of the invention not only contains ammonium polyphosphate as main flame retardant, also contains grape
Calciofon is as compound flame retardant, hence it is evident that improves the flame retarding efficiency of ammonium polyphosphate.
(2) calcium gluconate contained by expansion type fire retarding epoxide resin of the invention can be used as carbon source, but also as gas
Source.
(3) fire retardant contained by expansion type fire retarding epoxide resin of the invention be Halogen compound, in combustion without
Halogen gas release, avoids the injury to environment and human body.
(4) expansion type flame retardant epoxy resin preparation process of the invention is simple, and raw material are simple and easy to get, at low cost, has
Conducive to expanding production.
Specific embodiment
The present invention will be further described in detail with reference to the specific embodiments:
A kind of expansion type fire retarding epoxide resin, component and each component mass percent are as follows:
Epoxy resin 42.5%~85%；
Curing agent 5%~42.5%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%~35.5%, UL-94 vertical combustion rank is V-1
~V-0 grades.
Preferably, a kind of expansion type fire retarding epoxide resin, component and each component mass percent are as follows:
Epoxy resin 65%~75%；
Curing agent 15%~20%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin be 30.9%~35%, UL-94 vertical combustion rank be V-1~
V-0 grades.
The epoxy resin is E44 epoxy resin or E51 epoxy resin.
The curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and low molecular polyamides tree
Any one of rouge 650.
The ratio between ammonium polyphosphate and the mass fraction of calcium gluconate are in the ammonium polyphosphate and gluconic acid calcium complexes
4:1~10:1.
Preferably, ammonium polyphosphate and the quality of calcium gluconate point in the ammonium polyphosphate and gluconic acid calcium complexes
The ratio between number is 6:1~8:1.
Preferably, the expansion type fire retarding epoxide resin with a thickness of 3.2mm.
A kind of preparation method of expansion type fire retarding epoxide resin, the preparation method comprises the following steps:
1) epoxy resin, curing agent, ammonium polyphosphate and gluconic acid calcium complexes are weighed by each component mass percent；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
Embodiment 1
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 45 grams of epoxy resin, 45 grams of curing agent, 10 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E44 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate and Portugal
Contain 8 grams of ammonium polyphosphate and 2 grams of calcium gluconates in grape saccharic acid calcium complexes；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%, UL-94 vertical combustion rank is V-1 grades.
Embodiment 2
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 44 grams of epoxy resin, 44 grams of curing agent, 12 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E44 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate and Portugal
Contain 10.67 grams of ammonium polyphosphate and 1.33 grams of calcium gluconates in grape saccharic acid calcium complexes；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.0%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 3
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 42.5 grams of epoxy resin, 42.5 grams of curing agent, 15 grams of ammonium polyphosphate and Portugal are weighed
Grape saccharic acid calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate
With in gluconic acid calcium complexes contain 12.86 grams of ammonium polyphosphate and 2.14 grams of calcium gluconates；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 35.0%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 4
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 58.7 grams of epoxy resin, 29.3 grams of curing agent, 12 grams of ammonium polyphosphate and Portugal are weighed
Grape saccharic acid calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate
With in gluconic acid calcium complexes contain 10.5 grams of ammonium polyphosphate and 1.5 grams of calcium gluconates；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 30.9%, UL-94 vertical combustion rank is V-1 grades.
Embodiment 5
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 85 grams of epoxy resin, 5 grams of curing agent, 10 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E44 epoxy resin, and curing agent is diethylenetriamine, ammonium polyphosphate and calcium gluconate
Contain 8 grams of ammonium polyphosphate and 2 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 31.5%, UL-94 vertical combustion rank is V-1 grades.
Embodiment 6
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 85 grams of epoxy resin, 5 grams of curing agent, 10 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E44 epoxy resin, and curing agent is diethylenetriamine, ammonium polyphosphate and calcium gluconate
Contain 9.09 grams of ammonium polyphosphate and 0.91 gram of calcium gluconate in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 32%, UL-94 vertical combustion rank is V-1 grades.
Embodiment 7
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 83 grams of epoxy resin, 7 grams of curing agent, 10 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, ammonium polyphosphate and calcium gluconate
Contain 8.57 grams of ammonium polyphosphate and 1.43 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 32.5%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 8
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 80 grams of epoxy resin, 5 grams of curing agent, 15 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, ammonium polyphosphate and calcium gluconate
Contain 12.86 grams of ammonium polyphosphate and 2.14 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.9%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 9
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 80 grams of epoxy resin, 7 grams of curing agent, 13 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, ammonium polyphosphate and calcium gluconate
Contain 11.56 grams of ammonium polyphosphate and 1.44 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 34.5%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 10
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 80 grams of epoxy resin, 10 grams of curing agent, 10 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E44 epoxy resin, and curing agent is tetraethylenepentamine, ammonium polyphosphate and calcium gluconate
Contain 8 grams of ammonium polyphosphate and 2 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 31.9%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 11
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 76 grams of epoxy resin, 9 grams of curing agent, 15 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is triethylene tetramine, ammonium polyphosphate and calcium gluconate
Contain 12 grams of ammonium polyphosphate and 3 grams of calcium gluconates in compound；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.4%, UL-94 vertical combustion rank is V-0 grades.
Embodiment 12
A kind of preparation method of expansion type fire retarding epoxide resin comprising following steps:
1) each component mass percent is pressed, 72 grams of epoxy resin, 8 grams of curing agent, 20 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes；Wherein, epoxy resin is E51 epoxy resin, and curing agent is ethylenediamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 18 grams of ammonium polyphosphate and 2 grams of calcium gluconates in object；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, are stirred evenly, and vacuumized
Bubble is removed, level-one mixture is obtained；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then is controlled
Heating temperature processed is 100 DEG C and solidifies 2 hours.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.9%, UL-94 vertical combustion rank is V-0 grades.
Using expansion type fire retarding epoxide resin preparation method of the present invention, expansion type fire retarding epoxide resin sample obtained is through surveying
Examination, the results are shown in Table 1:
| Embodiment | Oxygen index (OI) (%) | UL-94 (grade) | Embodiment | Oxygen index (OI) (%) | UL-94 (grade) |
| Embodiment 1 | 29.0 | V-1 | Embodiment 7 | 32.5 | V-0 |
| Embodiment 2 | 33.0 | V-0 | Embodiment 8 | 33.9 | V-0 |
| Embodiment 3 | 35.0 | V-0 | Embodiment 9 | 34.5 | V-0 |
| Embodiment 4 | 30.9 | V-1 | Embodiment 10 | 31.9 | V-0 |
| Embodiment 5 | 31.5 | V-1 | Embodiment 11 | 33.4 | V-0 |
| Embodiment 6 | 32.0 | V-1 | Embodiment 12 | 33.9 | V-0 |
Above description should not have any restriction to protection scope of the present invention.
Claims (6)
1. a kind of expansion type fire retarding epoxide resin, it is characterised in that: its component and each component mass percent are as follows:
Epoxy resin 42.5%~85%；
Curing agent 5%~42.5%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%~35.5%, UL-94 vertical combustion rank is V-1~V-0
Grade；
In the ammonium polyphosphate and gluconic acid calcium complexes the ratio between mass fraction of ammonium polyphosphate and calcium gluconate be 4:1~
10:1。
2. a kind of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: its component and each component quality
Percentage are as follows:
Epoxy resin 65%~75%；
Curing agent 15%~20%；
Ammonium polyphosphate and gluconic acid calcium complexes 10%~15%；
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 30.9%~35%, UL-94 vertical combustion rank is V-1~V-0 grades.
3. a kind of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: the epoxy resin is E44
Epoxy resin or E51 epoxy resin.
4. a kind of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: the curing agent is second two
Any one of amine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and low-molecular-weight polyamide resin 650.
5. a kind of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: the ammonium polyphosphate and grape
The ratio between mass fraction of ammonium polyphosphate and calcium gluconate is 6:1~8:1 in saccharic acid calcium complexes.
6. a kind of preparation method of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: the preparation
Method the following steps are included:
1) epoxy resin, curing agent, ammonium polyphosphate and gluconic acid calcium complexes are weighed by each component mass percent；
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 °C of epoxy resin, are stirred evenly, and vacuumize removing
Bubble obtains level-one mixture；
3) curing agent is added in level-one mixture, stirring obtains second level mixture to uniform system is become rapidly；
4) second level mixture is injected into mold, be put into baking oven, first controlling heating temperature is 80 DEG C of solidifications 2 hours, then controls and add
Hot temperature is 100 DEG C and solidifies 2 hours.
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| CN116790157B (en) * | 2023-06-29 | 2024-05-07 | 华鼎国联四川电池材料有限公司 | Flame-retardant protective film based on polyethylene and intumescent flame retardant, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012078058A1 (en) * | 2010-12-10 | 2012-06-14 | Instytut Inżynierii Materiałów Polimerowych I Barwników | Flame-retardant epoxy resins and epoxy glass-reinforced laminates |
| CN104927577A (en) * | 2015-06-29 | 2015-09-23 | 青岛文晟汽车零部件有限公司 | Anti-corrosion weather-resistant epoxy resin paint for copper sculptures |
| CN106009040A (en) * | 2016-06-24 | 2016-10-12 | 福建师范大学 | Flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and preparation method of flame retardant |
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