CN107501864A - A kind of fire-retardant, high rigidity encapsulating material and its preparation method and application - Google Patents
A kind of fire-retardant, high rigidity encapsulating material and its preparation method and application Download PDFInfo
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- CN107501864A CN107501864A CN201710776984.6A CN201710776984A CN107501864A CN 107501864 A CN107501864 A CN 107501864A CN 201710776984 A CN201710776984 A CN 201710776984A CN 107501864 A CN107501864 A CN 107501864A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
-
- 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
- C08K2003/325—Calcium, strontium or barium phosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of fire-retardant, high rigidity encapsulating material and its preparation method and application, the encapsulating material includes according to the raw material of parts by weight：25 35 parts of makrolon, 33 41 parts of epoxy resin E21,11 19 parts of cumyl peroxide, 37 parts of isomerous tridecanol polyoxyethylene ether, 20 30 parts of apatite, 12 20 parts of polyethylene glycol.By makrolon, apatite crushing, sieving, then stirred with cumyl peroxide solution Hybrid Heating；Add polyethylene glycol and epoxy resin E21 heating stirrings；Then the heating of addition isomerous tridecanol polyoxyethylene ether solution, melting extrusion, injection molding produce.Encapsulating material produced by the present invention, there is high anti-flammability, heat resistance, resistance to acids and bases, hydrolytic resistance and ground water imbibition, effectively raise the hardness of product；It is high for electronic package material, flame retarding efficiency.Raw material of the present invention is simple, and preparation process is simple, light, environmentally friendly, safe and non-toxic, does not produce poisonous and harmful substances during production, cost is low, suitable for industrialized production.
Description
Technical field
The present invention relates to encapsulating material technical field, specifically a kind of fire-retardant, high rigidity encapsulating material and its preparation side
Method and application.
Background technology
Epoxy resin is one of most widely used matrix resin in polymer matrix composite, by the change with epoxy radicals
Prepared by compound carries out polycondensation reaction with multi-hydroxy or polyol compound product, has excellent caking property, chemically-resistant
Corrosivity, electrical insulation properties, mechanical property, and it is easy to process, that shrinkage factor is low, linear expansion coefficient is small and cost is cheap etc. is excellent
Point, it is widely used in the encapsulation of the electronic components such as piezo-resistance, ceramic capacitor, diode, triode.
But due to the limited oxygen index of epoxy resin（LOI）It is relatively low, belong to combustible material, it is therefore desirable to it is carried out fire-retardant
Processing.Generally, the method for improving ethoxyline resin antiflaming is to introduce halogen-containing fire retardant in the epoxy, and coordinates such as three
The flame retardant of two antimony classes is aoxidized, so as to assign epoxy resin excellent flame retardant property.But chlorine-containing flame retardant and antimony oxide
The flame retardant of class can produce bioxin again in burning（Dioxin）Deng toxic smoke and corrosive gas（Such as hydrogen bromide）, serious shadow
The healthy and for the survival of mankind environment of the mankind is rung.In addition, use of the hardness of encapsulating material to electronic component have it is larger
Effect, relatively low hardness can cause the mechanical performance of encapsulating material to decline, reduce the product quality of electronic component.
The content of the invention
It is an object of the invention to provide a kind of fire-retardant, high rigidity encapsulating material and its preparation method and application, with solution
The problem of being proposed in certainly above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of fire-retardant, high rigidity encapsulating material, includes according to the raw material of parts by weight：Makrolon 25-35 parts, epoxy resin
It is E21 33-41 parts, cumyl peroxide 11-19 parts, isomerous tridecanol polyoxyethylene ether 3-7 parts, apatite 20-30 parts, poly-
Ethylene glycol 12-20 parts.
As the further scheme of the present invention：Fire-retardant, high rigidity the encapsulating material, according to the raw material bag of parts by weight
Include：Makrolon 28-32 parts, epoxy resin E21 35-39 parts, cumyl peroxide 13-17 parts, isomerous tridecanol polyoxy second
Alkene ether 4-6 parts, apatite 22-28 parts, polyethylene glycol 14-18 parts.
As the further scheme of the present invention：Fire-retardant, high rigidity the encapsulating material, according to the raw material bag of parts by weight
Include：30 parts of makrolon, 37 parts of epoxy resin E21,15 parts of cumyl peroxide, 5 parts of isomerous tridecanol polyoxyethylene ether,
25 parts of apatite, 16 parts of polyethylene glycol.
A kind of preparation method of fire-retardant, high rigidity encapsulating material, comprises the following steps：
1）15-17 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8-9 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made；
2）By makrolon, apatite crushing, 100-150 mesh sieves are crossed, then mixes, is heated to cumyl peroxide solution
62-66 DEG C and stir process 1.5-1.8h at such a temperature；Polyethylene glycol and epoxy resin E21 are added, is warming up to 70-72
DEG C, and stir process 45-50min at such a temperature；Then isomerous tridecanol polyoxyethylene ether solution is added, and at 92-96 DEG C
At a temperature of stir 35-40min, mixture A is made；
3）Mixture A is warming up to 135-140 DEG C and at such a temperature stir process 25-30min, then in 165-170 DEG C of temperature
The lower stirring 25-30min of degree, is made mixture B；
4）Mixture B is produced through melting extrusion, injection molding.
As the further scheme of the present invention：Step 2）In, mixing speed 150-180r/min.
As the further scheme of the present invention：Step 2）In, mixed with cumyl peroxide solution, be heated to 64 DEG C.
As the further scheme of the present invention：Step 2）In, isomerous tridecanol polyoxyethylene ether solution is added, and at 94 DEG C
At a temperature of stir 35-40min.
As the further scheme of the present invention：Step 3）In, mixing speed 250-280r/min.
As the further scheme of the present invention：Step 3）In, mixture A is warming up to 138 DEG C and stirred at such a temperature
25-30min is handled, then 25-30min is stirred at a temperature of 168 DEG C, mixture B is made.
Another object of the present invention is to provide the application of the encapsulating material in the electronic device.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention using encapsulating material made from above-mentioned raw materials and technique, have high anti-flammability, heat resistance, resistance to acids and bases,
Hydrolytic resistance and ground water imbibition, effectively raise the hardness of product；For electronic package material, flame retarding efficiency is high, without
Add other fire retardants again, you can realize the excellent fire-retardant persistence of electronic package material, heat resistance, resistance to acids and bases and electrically
Energy.Raw material of the present invention is simple, and preparation process is simple, light, environmentally friendly, safe and non-toxic, does not produce poisonous and harmful substances, cost during production
It is low, suitable for industrialized production.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of fire-retardant, high rigidity encapsulating material, including following raw material：Makrolon 25kg, asphalt mixtures modified by epoxy resin
Fat E21 33kg, cumyl peroxide 11kg, isomerous tridecanol polyoxyethylene ether 3kg, apatite 20kg, polyethylene glycol
12kg。
15 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made.By poly- carbon
Acid esters, apatite crush, cross 100 mesh sieves, are then mixed with cumyl peroxide solution, are heated to 62 DEG C and at such a temperature
Stir process 1.5h；Polyethylene glycol and epoxy resin E21 are added, is warming up to 70 DEG C, and stir process at such a temperature
45min；Then isomerous tridecanol polyoxyethylene ether solution is added, and 35min is stirred at a temperature of 92 DEG C, mixture A is made；
In above-mentioned steps, mixing speed 150r/min.Mixture A is warming up to 135 DEG C and at such a temperature stir process 25min,
25min is stirred at a temperature of 165 DEG C again, mixture B is made；In above-mentioned steps, mixing speed 250r/min.By mixture
B produces through melting extrusion, injection molding.
Embodiment 2
In the embodiment of the present invention, a kind of fire-retardant, high rigidity encapsulating material, including following raw material：Makrolon 35kg, asphalt mixtures modified by epoxy resin
Fat E21 41kg, cumyl peroxide 19kg, isomerous tridecanol polyoxyethylene ether 7kg, apatite 30kg, polyethylene glycol
20kg。
17 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 9 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made.By poly- carbon
Acid esters, apatite crush, cross 150 mesh sieves, are then mixed with cumyl peroxide solution, are heated to 66 DEG C and at such a temperature
Stir process 1.8h；Polyethylene glycol and epoxy resin E21 are added, is warming up to 72 DEG C, and stir process at such a temperature
50min；Then isomerous tridecanol polyoxyethylene ether solution is added, and 40min is stirred at a temperature of 96 DEG C, mixture A is made；
In above-mentioned steps, mixing speed 180r/min.Mixture A is warming up to 140 DEG C and at such a temperature stir process 30min,
30min is stirred at a temperature of 170 DEG C again, mixture B is made；In above-mentioned steps, mixing speed 280r/min.By mixture
B produces through melting extrusion, injection molding.
Embodiment 3
In the embodiment of the present invention, a kind of fire-retardant, high rigidity encapsulating material, including following raw material：Makrolon 28kg, asphalt mixtures modified by epoxy resin
Fat E21 35kg, cumyl peroxide 13kg, isomerous tridecanol polyoxyethylene ether 4kg, apatite 22kg, polyethylene glycol
14kg。
16 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8.5 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made.Will be poly-
Carbonic ester, apatite crush, cross 120 mesh sieves, are then mixed with cumyl peroxide solution, are heated to 64 DEG C and in the temperature
Lower stir process 1.8h；Polyethylene glycol and epoxy resin E21 are added, is warming up to 71 DEG C, and stir process at such a temperature
50min；Then isomerous tridecanol polyoxyethylene ether solution is added, and 40min is stirred at a temperature of 94 DEG C, mixture A is made；
In above-mentioned steps, mixing speed 180r/min.Mixture A is warming up to 138 DEG C and at such a temperature stir process 30min,
30min is stirred at a temperature of 168 DEG C again, mixture B is made；In above-mentioned steps, mixing speed 280r/min.By mixture
B produces through melting extrusion, injection molding.
Embodiment 4
In the embodiment of the present invention, a kind of fire-retardant, high rigidity encapsulating material, including following raw material：Makrolon 32kg, asphalt mixtures modified by epoxy resin
Fat E21 39kg, cumyl peroxide 17kg, isomerous tridecanol polyoxyethylene ether 6kg, apatite 28kg, polyethylene glycol
18kg。
16 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8.5 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made.Will be poly-
Carbonic ester, apatite crush, cross 120 mesh sieves, are then mixed with cumyl peroxide solution, are heated to 64 DEG C and in the temperature
Lower stir process 1.8h；Polyethylene glycol and epoxy resin E21 are added, is warming up to 71 DEG C, and stir process at such a temperature
50min；Then isomerous tridecanol polyoxyethylene ether solution is added, and 40min is stirred at a temperature of 94 DEG C, mixture A is made；
In above-mentioned steps, mixing speed 180r/min.Mixture A is warming up to 138 DEG C and at such a temperature stir process 30min,
30min is stirred at a temperature of 168 DEG C again, mixture B is made；In above-mentioned steps, mixing speed 280r/min.By mixture
B produces through melting extrusion, injection molding.
Embodiment 5
In the embodiment of the present invention, a kind of fire-retardant, high rigidity encapsulating material, including following raw material：Makrolon 30kg, asphalt mixtures modified by epoxy resin
Fat E21 37kg, cumyl peroxide 15kg, isomerous tridecanol polyoxyethylene ether 5kg, apatite 25kg, polyethylene glycol
16kg。
16 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8.5 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made.Will be poly-
Carbonic ester, apatite crush, cross 120 mesh sieves, are then mixed with cumyl peroxide solution, are heated to 64 DEG C and in the temperature
Lower stir process 1.8h；Polyethylene glycol and epoxy resin E21 are added, is warming up to 71 DEG C, and stir process at such a temperature
50min；Then isomerous tridecanol polyoxyethylene ether solution is added, and 40min is stirred at a temperature of 94 DEG C, mixture A is made；
In above-mentioned steps, mixing speed 180r/min.Mixture A is warming up to 138 DEG C and at such a temperature stir process 30min,
30min is stirred at a temperature of 168 DEG C again, mixture B is made；In above-mentioned steps, mixing speed 280r/min.By mixture
B produces through melting extrusion, injection molding.
Comparative example 1
In addition to cumyl peroxide is not contained, its material composition is consistent with embodiment 5 with preparation technology.
Comparative example 2
In addition to isomerous tridecanol polyoxyethylene ether is not contained, its material composition is consistent with embodiment 5 with preparation technology.
Comparative example 3
Each raw material is directly mixed to prepare mixture A, mixture A is warming up to 138 DEG C and at such a temperature stir process
30min, then 30min is stirred at a temperature of 168 DEG C, mixture B is made；In above-mentioned steps, mixing speed 280r/min.Will
Mixture B produces through melting extrusion, injection molding.Its material composition is consistent with embodiment 5.
Embodiment 1-5 and comparative example 1-3 encapsulating material are tested.Test result is as shown in table 1：
Table 1
| Anti-flammability | Anti-flammability：5 sample total burning times（s） | Shore hardness（A） | |
| Embodiment 1 | v-0 | 50 | 63 |
| Embodiment 2 | v-0 | 45 | 65 |
| Embodiment 3 | v-0 | 25 | 68 |
| Embodiment 4 | v-0 | 22 | 69 |
| Embodiment 5 | v-0 | 15 | 71 |
| Comparative example 1 | v-2 | 150 | 55 |
| Comparative example 2 | v-2 | 165 | 40 |
| Comparative example 3 | v-1 | 120 | 42 |
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of spirit or essential attributes from the present invention, the present invention can be realized in other specific forms.Therefore, no matter from which
From the point of view of a bit, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention will by appended right
Ask rather than described above limits, it is intended that all changes in the implication and scope of the equivalency of claim will be fallen
Include in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (10)
1. a kind of fire-retardant, high rigidity encapsulating material, it is characterised in that include according to the raw material of parts by weight：Makrolon 25-35
Part, epoxy resin E21 33-41 parts, cumyl peroxide 11-19 parts, isomerous tridecanol polyoxyethylene ether 3-7 parts, apatite
20-30 parts, polyethylene glycol 12-20 parts.
2. fire-retardant, high rigidity encapsulating material according to claim 1, it is characterised in that according to the raw material bag of parts by weight
Include：Makrolon 28-32 parts, epoxy resin E21 35-39 parts, cumyl peroxide 13-17 parts, isomerous tridecanol polyoxy second
Alkene ether 4-6 parts, apatite 22-28 parts, polyethylene glycol 14-18 parts.
3. fire-retardant, high rigidity encapsulating material according to claim 1, it is characterised in that according to the raw material bag of parts by weight
Include：30 parts of makrolon, 37 parts of epoxy resin E21,15 parts of cumyl peroxide, 5 parts of isomerous tridecanol polyoxyethylene ether,
25 parts of apatite, 16 parts of polyethylene glycol.
A kind of 4. preparation method of fire-retardant, high rigidity encapsulating material as described in claim 1-3 is any, it is characterised in that
Comprise the following steps：
1）15-17 times of ethanol of cumyl peroxide and its quality is mixed, cumyl peroxide solution is made；By isomery
The deionized water of 8-9 times of tridecanol polyoxyethylene ether and its quality mixes, and isomerous tridecanol polyoxyethylene ether solution is made；
2）By makrolon, apatite crushing, 100-150 mesh sieves are crossed, then mixes, is heated to cumyl peroxide solution
62-66 DEG C and stir process 1.5-1.8h at such a temperature；Polyethylene glycol and epoxy resin E21 are added, is warming up to 70-72
DEG C, and stir process 45-50min at such a temperature；Then isomerous tridecanol polyoxyethylene ether solution is added, and at 92-96 DEG C
At a temperature of stir 35-40min, mixture A is made；
3）Mixture A is warming up to 135-140 DEG C and at such a temperature stir process 25-30min, then in 165-170 DEG C of temperature
The lower stirring 25-30min of degree, is made mixture B；
4）Mixture B is produced through melting extrusion, injection molding.
5. the preparation method of fire-retardant, high rigidity encapsulating material according to claim 4, it is characterised in that step 2）In,
Mixing speed is 150-180r/min.
6. the preparation method of fire-retardant, high rigidity encapsulating material according to claim 4, it is characterised in that step 2）In,
Mixed with cumyl peroxide solution, be heated to 64 DEG C.
7. the preparation method of fire-retardant, high rigidity encapsulating material according to claim 4, it is characterised in that step 2）In,
Isomerous tridecanol polyoxyethylene ether solution is added, and 35-40min is stirred at a temperature of 94 DEG C.
8. the preparation method of fire-retardant, high rigidity encapsulating material according to claim 4, it is characterised in that step 3）In,
Mixing speed is 250-280r/min.
9. the preparation method of fire-retardant, high rigidity encapsulating material according to claim 4, it is characterised in that step 3）In,
Mixture A is warming up to 138 DEG C and at such a temperature stir process 25-30min, then 25- is stirred at a temperature of 168 DEG C
30min, mixture B is made.
10. the application of encapsulating material in the electronic device as described in claim 1-3 is any.
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| CN103694644A (en) * | 2013-12-30 | 2014-04-02 | 景旺电子科技(龙川)有限公司 | Epoxy resin composition, metal-based copper-clad plate and manufacturing method thereof |
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Application publication date: 20171222 |