CN108084660A - 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
- Publication number
- CN108084660A CN108084660A CN201711439481.6A CN201711439481A CN108084660A CN 108084660 A CN108084660 A CN 108084660A CN 201711439481 A CN201711439481 A CN 201711439481A CN 108084660 A CN108084660 A CN 108084660A
- Authority
- CN
- China
- Prior art keywords
- ammonium polyphosphate
- expansion type
- fire retarding
- type fire
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of expansion type fire retarding epoxide resin, component and each component mass percent are: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 in the ammonium polyphosphate and gluconic acid calcium complexes:1~10:1;The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%~35.5%, UL, 94 vertical combustion ranks are 0 grade of 1~V of V.The invention also discloses its preparation methods.Present invention employs ammonium polyphosphate and gluconic acid calcium complexes as expansion type flame retardant fire retarding epoxide resin, 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 technology
Epoxy resin cured product is due to having many advantages, such as that mechanical strength height, insulating properties, thermal stability be good, chemical 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, it is impossible to meet and be wanted 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, is prepared
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 add 21% ammonium polyphosphate, the vertical combustion of epoxy resin
Rank is stepless;After ammonium polyphosphate and cuprous oxide compound, 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, so as to reduce cost.
The content 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 present invention uses following technical scheme:
A kind of expansion type fire retarding epoxide resin, component and each component mass percent are:
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 combustions rank is V-1~V-
0 grade.
Preferably, a kind of expansion type fire retarding epoxide resin, component and each component mass percent are:
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 combustions rank is V-1~V-0
Grade.
The epoxy resin is E44 epoxy resin or E51 epoxy resin.
The curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and low-molecular-weight polyamide resin
Any one of 650.
The ratio between mass fraction of ammonium polyphosphate and calcium gluconate is 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 thickness of the expansion type fire retarding epoxide resin is 3.2mm.
A kind of preparation method of expansion type fire retarding epoxide resin, the preparation method comprise 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The present invention employs ammonium polyphosphate and gluconic acid calcium complexes as expansion type flame-retarding using above technical scheme
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, has the following advantages:
(1) expansion type fire retarding epoxide resin of the invention not only contains ammonium polyphosphate as main flame retardant, also contains gluconic acid
Calcium 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 source of the gas.
(3) fire retardant contained by expansion type fire retarding epoxide resin of the invention is Halogen compound, in combustion without halogen
Gas discharges, and 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, are 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:
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 combustions rank is V-1~V-
0 grade.
Preferably, a kind of expansion type fire retarding epoxide resin, component and each component mass percent are:
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 combustions rank is V-1~V-0
Grade.
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 fat 650.
The ratio between mass fraction of ammonium polyphosphate and calcium gluconate is 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 thickness of the expansion type fire retarding epoxide resin is 3.2mm.
A kind of preparation method of expansion type fire retarding epoxide resin, the preparation method comprise 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
Embodiment 1
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 45 grams of epoxy resin, 45 grams of curing agent, 10 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E44 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate and glucose
Contain 8 grams of ammonium polyphosphate and 2 grams of calcium gluconates in sour calcium complexes;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 29.0%, UL-94 vertical combustions rank is V-1 grades.
Embodiment 2
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 44 grams of epoxy resin, 44 grams of curing agent, 12 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E44 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate and glucose
Contain 10.67 grams of ammonium polyphosphate and 1.33 grams of calcium gluconates in sour calcium complexes;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.0%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 3
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 42.5 grams of epoxy resin, 42.5 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 low molecular polyamides 650, ammonium polyphosphate and Portugal
Contain 12.86 grams of ammonium polyphosphate and 2.14 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 35.0%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 4
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 58.7 grams of epoxy resin, 29.3 grams of curing agent, 12 grams of ammonium polyphosphate and glucose are weighed
Sour calcium complexes;Wherein, epoxy resin is E51 epoxy resin, and curing agent is low molecular polyamides 650, ammonium polyphosphate and Portugal
Contain 10.5 grams of ammonium polyphosphate and 1.5 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 30.9%, UL-94 vertical combustions rank is V-1 grades.
Embodiment 5
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 85 grams of epoxy resin, 5 grams of curing agent, 10 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E44 epoxy resin, and curing agent is diethylenetriamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 8 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 31.5%, UL-94 vertical combustions rank is V-1 grades.
Embodiment 6
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 85 grams of epoxy resin, 5 grams of curing agent, 10 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E44 epoxy resin, and curing agent is diethylenetriamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 9.09 grams of ammonium polyphosphate and 0.91 gram of calcium gluconate in object;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 32%, UL-94 vertical combustions rank is V-1 grades.
Embodiment 7
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 83 grams of epoxy resin, 7 grams of curing agent, 10 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 8.57 grams of ammonium polyphosphate and 1.43 grams of calcium gluconates in object;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 32.5%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 8
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 80 grams of epoxy resin, 5 grams of curing agent, 15 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 12.86 grams of ammonium polyphosphate and 2.14 grams of calcium gluconates in object;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.9%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 9
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 80 grams of epoxy resin, 7 grams of curing agent, 13 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E51 epoxy resin, and curing agent is diethylenetriamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 11.56 grams of ammonium polyphosphate and 1.44 grams of calcium gluconates in object;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 34.5%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 10
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 80 grams of epoxy resin, 10 grams of curing agent, 10 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E44 epoxy resin, and curing agent is tetraethylenepentamine, and ammonium polyphosphate and calcium gluconate are compound
Contain 8 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, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 31.9%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 11
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 76 grams of epoxy resin, 9 grams of curing agent, 15 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E51 epoxy resin, and curing agent is triethylene tetramine, and ammonium polyphosphate and calcium gluconate are compound
Contain 12 grams of ammonium polyphosphate and 3 grams of calcium gluconates in object;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.4%, UL-94 vertical combustions rank is V-0 grades.
Embodiment 12
A kind of preparation method of expansion type fire retarding epoxide resin, comprises the following steps:
1) by each component mass percent, 72 grams of epoxy resin, 8 grams of curing agent, 20 grams of ammonium polyphosphate and calcium gluconate are weighed
Compound;Wherein, epoxy resin is E51 epoxy resin, and curing agent is ethylenediamine, in ammonium polyphosphate and gluconic acid calcium complexes
Contain 18 grams of ammonium polyphosphate and 2 grams of calcium gluconates;
2) ammonium polyphosphate and gluconic acid calcium complexes are added in 60 DEG C of epoxy resin, stirred evenly, and vacuumize removing
Bubble obtains level-one mixture;
3) curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4) by two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
The oxygen index (OI) of the expansion type fire retarding epoxide resin is that 33.9%, UL-94 vertical combustions 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 protection scope of the present invention any restriction.
Claims (7)
1. a kind of expansion type fire retarding epoxide resin, it is characterised in that:Its component and each component mass percent are:
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 combustions rank is V-1~V-0
Grade.
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 is:
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 combustions 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 4 in saccharic acid calcium complexes:1~10:1.
6. a kind of expansion type fire retarding epoxide resin according to claim 5, it is characterised in that:The ammonium polyphosphate and grape
The ratio between mass fraction of ammonium polyphosphate and calcium gluconate is 6 in saccharic acid calcium complexes:1~8:1.
7. a kind of preparation method of expansion type fire retarding epoxide resin according to claim 1, it is characterised in that: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 °C of epoxy resin, stirred evenly, and vacuumizes removing
Bubble obtains level-one mixture;
3)Curing agent is added in level-one mixture, rapid stirring obtains two level mixture to homogeneous system is become;
4)By two level mixture inject mold, be put into baking oven, first control heating temperature for 80 DEG C cure 2 it is small when, then control add
When hot temperature is that 100 DEG C of curings 2 are small.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711439481.6A CN108084660B (en) | 2017-12-27 | 2017-12-27 | A kind of expansion type fire retarding epoxide resin and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711439481.6A CN108084660B (en) | 2017-12-27 | 2017-12-27 | A kind of expansion type fire retarding epoxide resin and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108084660A true CN108084660A (en) | 2018-05-29 |
CN108084660B CN108084660B (en) | 2019-10-18 |
Family
ID=62179572
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711439481.6A Active CN108084660B (en) | 2017-12-27 | 2017-12-27 | A kind of expansion type fire retarding epoxide resin and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108084660B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108864793A (en) * | 2018-06-21 | 2018-11-23 | 太原理工大学 | A kind of expandable flame retardant coating and preparation method thereof |
CN116790157A (en) * | 2023-06-29 | 2023-09-22 | 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 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
-
2017
- 2017-12-27 CN CN201711439481.6A patent/CN108084660B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108864793A (en) * | 2018-06-21 | 2018-11-23 | 太原理工大学 | A kind of expandable flame retardant coating and preparation method thereof |
CN116790157A (en) * | 2023-06-29 | 2023-09-22 | 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 |
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 |
Also Published As
Publication number | Publication date |
---|---|
CN108084660B (en) | 2019-10-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Zhu et al. | Synthesis of an effective bio-based flame-retardant curing agent and its application in epoxy resin: Curing behavior, thermal stability and flame retardancy | |
CN109942891B (en) | Phosphorus-nitrogen-zinc two-dimensional supermolecule coated molybdenum disulfide hybrid flame retardant and application thereof | |
CN105440652B (en) | A kind of flame retardant thermoplastic polyurethane elastomer and preparation method thereof | |
CN102276837A (en) | Halogen-free phosphorus-containing flame retardant polyimide resin composite and preparation method thereof | |
KR100929842B1 (en) | Pultrusion anti fire frp products | |
JP2018012837A (en) | Flame retardant resin composition, thermosetting resin composition, composite metal substrate and flame retardant electronic material | |
CN108084660B (en) | A kind of expansion type fire retarding epoxide resin and preparation method thereof | |
CN112250985B (en) | Halogen-free flame-retardant ABS composition and preparation method and application thereof | |
CN109096471B (en) | P-N-Si synergistic flame-retardant epoxy resin curing agent and preparation method thereof | |
CN110982465B (en) | Efficient halogen-free flame-retardant epoxy adhesive and preparation method thereof | |
CN104479350A (en) | Halogen-free flame-retarded polycaprolactam compound with low smoke and extremely low odor | |
CN113667277A (en) | Low-heat-release, low-smoke and high-flame-retardant epoxy resin material and preparation method thereof | |
CN109266007A (en) | Expandable flame retardant room temperature vulcanized silicone rubber formula and expandable flame retardant room temperature vulcanized silicone rubber | |
CN112679545B (en) | Melamine-based nitrogen-phosphorus-containing compound, preparation method and application thereof, and flame-retardant epoxy resin composition thereof | |
CN115058093A (en) | Environment-friendly PVC plastic film and production process thereof | |
CN111777912B (en) | Flame-retardant and flexible epoxy resin composition and preparation method thereof | |
KR20220018432A (en) | Flame retardant plastic based on adenosine triphosphate and polyethylene | |
CN106854370B (en) | A kind of supermolecule flame-proof silicon rubber and preparation method thereof | |
CN106243629B (en) | A kind of preparation method and application of fire-retardant modified epoxy resin | |
CN106633752B (en) | A kind of halogen-free flame retardant PC ABS alloy material and its preparation method and application | |
CN106398150A (en) | A halogen-free flame-retardant thermosetting type resin composite material and a preparing method thereof | |
CN108485192B (en) | N-P synergistic high-flame-retardant epoxy resin composition with excellent flexibility and preparation method thereof | |
CN106519653A (en) | Novel efficient flame-retarded polyamide and preparation method thereof | |
CN108485056B (en) | Low-emigration halogen-free flame-retardant continuous long glass fiber reinforced polypropylene material and preparation method thereof | |
CN104829943A (en) | Fumed-silica-containing intumescent polypropylene flame retardant and preparation method of flame retardant |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |