CN102719067B - High-performance fiberglass reinforced plastic composite material and preparation method thereof - Google Patents
High-performance fiberglass reinforced plastic composite material and preparation method thereof Download PDFInfo
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- CN102719067B CN102719067B CN201210218055.0A CN201210218055A CN102719067B CN 102719067 B CN102719067 B CN 102719067B CN 201210218055 A CN201210218055 A CN 201210218055A CN 102719067 B CN102719067 B CN 102719067B
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Abstract
The invention provides a high-performance fiberglass reinforced plastic composite material and a preparation method thereof. The high-performance fiberglass reinforced plastic composite material consists of the following components in percentage by weight: 50 to 80 percent of dicyclopentadiene, 10 to 30 percent of hydrogen peroxide, 1 to 3 percent of potassium oxide, 0.1 to 0.5 percent of tungsten hexachloride, 1 to 5 percent of fire retardant, 2 to 4 percent of nano filler, 1 to 8 percent of glass fiber and 1 to 3 percent of metal filler. Hydrogen peroxide, fire retardant and potassium oxide are added into dicyclopentadiene, so that the softening temperature of the fiberglass reinforced plastic composite material can be increased and is more than 150 DGE C.
Description
Technical field
The present invention relates to a kind of matrix material and preparation method thereof, relate in particular to a kind of high performance polyester glass composite material and preparation method thereof.
Background technology
Fiberglass reinforced plastic matrix material generally refers to a kind of chemically composited material obtaining with glass fiber reinforced unsaturated polyester resin.Fiberglass reinforced plastic matrix material has light weight and hard, non-conductive, physical strength advantages of higher.But common fiberglass reinforced plastic exists flexural strength low, softening temperature is lower below 90 ℃.Be difficult to meet the requirement that some special occasions are used, as aerospace, automobile, building, body-building apparatus etc.
Summary of the invention
In sum, the high performance fiberglass reinforced plastic matrix material that provides a kind of softening temperature high is provided in the present invention.
A kind of high performance fiberglass reinforced plastic matrix material, component by following weight percent forms: the tungsten hexachloride 0.1-0.5% of dicyclopentadiene 50-80%, hydrogen peroxide 10-30%, potassium oxide 1-3%, phenol modification, fire retardant 1-5%, Nano filling 2-4%, glass fibre 3-8%, metallic stuffing 1-3%, this fiberglass reinforced plastic matrix material softening temperature is between 155-165 ℃.
Preferably, the weight percent of described hydrogen peroxide is 18-22%, 25-30%, 28-30%.
Preferably, the weight percent of described dicyclopentadiene is 60-65%, 73%-80%.
Preferably, described metallic stuffing is one or more in copper powder, iron powder or the tungsten powder of fineness between 200-500 order.
Preferably, the fineness of described metallic stuffing is 350 orders.
Preferably, described Nano filling is at least one in nano silicon or nano-calcium carbonate.
Preferably, the thickness of the firm matrix material of described polyester glass is 13-20mm.
Preferably, the shore hardness of described fiberglass reinforced plastic matrix material is 98-108D, and flexural strength is 185-195MPa, and resistance to impact shock is 260-285KJ/m
2.
A high performance fiberglass reinforced plastic matrix material, is comprised of the component of following weight percent:
Metallic stuffing 2.6%, 3%, 2.6%, the value of said components and be 100%.
The present invention is necessary to provide a kind of method of preparing above-mentioned fiberglass reinforced plastic matrix material, mainly comprises the following steps:
Prepare resin sheet: in temperature, be under 30-60 ℃ of condition, by the dicyclopentadiene of 35-50% weight, the hydrogen peroxide of 10-30% weight, the tungsten hexachloride of the phenol modification of 0.1-0.5% weight and the glass fibre of 1-4% weight add in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 160-250 ℃, at the fire retardant that continues to add under the prerequisite stirring 1-5% weight, 2-4% weight Nano filling, 1-3% weight potassium oxide, continue stirring reaction 6-8 hour, obtain unsaturated polyester resin, then this resin treatment is become to unsaturated polyester resin sheet,
Preimpregnated glass fibre cloth: get the metallic stuffing of 1-3% weight and mix with 15-30% weight dicyclopentadiene unsaturated polyester, then add the glasscloth that 1-4% weight is woven into by glass fibre to carry out preimpregnation; After preimpregnation, glasscloth is carried out to drying treatment under 130-150 ℃ of environment, obtain preimpregnated glass fibre cloth;
Prepare fiberglass reinforced plastic matrix material: some above-mentioned unsaturated polyester resin sheets and glasscloth are prepared and formed high performance fiberglass reinforced plastic matrix material by mould pressing process.
Fiberglass reinforced plastic matrix material of the present invention, adds potassium oxide can react generation potassium hydroxide, has the effect of thickening.By adding peroxidation Hydrogen Energy effectively to improve the softening temperature of this matrix material, can improve the softening temperature of this fiberglass reinforced plastic matrix material.
Embodiment
Below in conjunction with some embodiments, moiety of high performance fiberglass reinforced plastic matrix material of the present invention and preparation method thereof is further described.Specific embodiment is for further describing the present invention, non-limiting protection scope of the present invention.
The firm matrix material of high performance polyester glass of the present invention is comprised of dicyclopentadiene, hydrogen peroxide, catalyzer, thickening material, nano-calcium carbonate, glass fibre and metallic stuffing, the weight percent of each component is: the tungsten hexachloride 0.1-0.5% of dicyclopentadiene 50-80%, hydrogen peroxide 10-30%, potassium oxide 1-3%, phenol modification, fire retardant 1-5%, Nano filling 2-4%, glass fibre 1-8%, metallic stuffing 1-3%, the value of said components and be 100%.
Wherein, the weight percent of described hydrogen peroxide is 18-25%, 25-28%, 28-30%; The weight percent of described dicyclopentadiene is 60-65%, 75%-80%; When the weight percent of described glass fibre is 3-5%, the softening temperature of the firm matrix material of polyester glass preparing can reach 160 ℃ and more than.
Dicyclopentadiene, by adding hydrogen peroxide, can generate bicyclopentadiene dioxide by the dicyclopentadiene reaction of part.So polydicyclopentadiene resin mixes and includes bicyclopentadiene dioxide, thereby has improved the softening temperature of fiberglass reinforced plastic matrix material, adds fire retardant and potassium oxide to improve the softening temperature of this matrix material simultaneously.And this potassium oxide can react generation potassium hydroxide, has thickening power.
Nano filling, glass fibre, metallic stuffing be for strengthening the hardness of this matrix material, the thickening rate of the adjustable dicyclopentadiene of Nano filling in addition, thus can promote being uniformly distributed of glass fibre, Nano filling and metallic stuffing of the inside of matrix material.The tungsten hexachloride of described phenol modification is for catalysis dicyclopentadiene generation chemical reaction.
The preparation method of the tungsten hexachloride of phenol modification of the present invention is: tert.-butyl phenol is placed in to reactor, vacuumize and pour nitrogen by the air in reactor and steam discharge simultaneously, then add toluene, tungsten hexachloride, under the condition of 85 ℃ of left and right, back flow reaction is 18 hours, can obtain the tungsten hexachloride of phenol modification.The trade mark of described tert.-butyl phenol is 1010, is selected from Ningbo gold Hai Yabao.
Below in conjunction with specific embodiment, each component concentration and the preparation method of the firm matrix material of high-performance polyester glass of the present invention are described in detail:
Embodiment 1
Prepare vibrin sheet: in temperature, be under 30 ℃ of conditions, the hydrogen peroxide of 50kg dicyclopentadiene, 18kg, the tungsten hexachloride of 0.3kg phenol modification and the glass fibre of 2.7kg are added in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 160 ℃ of left and right, continuing to add 4kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 3kg nano silicon, 2kg potassium oxide, continue stirring reaction about 6 hours, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 2mm is standby.
Preimpregnated glass fibre cloth: getting 3kg fineness is 500 object iron powders and copper powder mixture, then said mixture is mixed with 15kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 2kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 150 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 4 layers of unsaturated polyester sheet and 4 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 13mm.
Embodiment 2
Prepare vibrin sheet: in temperature, be under 40 ℃ of conditions, the hydrogen peroxide of 35kg dicyclopentadiene, 30kg, the tungsten hexachloride of 0.5kg phenol modification and the glass fibre of 4kg are added in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 200 ℃ of left and right, continuing to add 5kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 4kg nano silicon, 1.5kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 3mm is standby.
Preimpregnated glass fibre cloth: getting 1kg fineness is 500 object iron powders and copper powder mixture, then said mixture is mixed with 17kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 2kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 150 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 4 layers of unsaturated polyester sheet and 4 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 14mm.
Embodiment 3
Prepare vibrin sheet: in temperature, be under 60 ℃ of conditions, by 50kg dicyclopentadiene, the hydrogen peroxide of 10kg, the tungsten hexachloride of 0.3kg phenol modification and the glass fibre of 2kg add in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 250 ℃ of left and right, continuing to add 2kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 1.7kg nano-calcium carbonate, 1kg silicon-dioxide, 1kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 1mm is standby.
Preimpregnated glass fibre cloth: getting 1kg fineness is 350 object iron powders, then said mixture is mixed with 30kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 1kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 130 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 9 layers of unsaturated polyester sheet and 7 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 15mm.
Embodiment 4
Prepare vibrin sheet: in temperature, be under 60 ℃ of conditions, the hydrogen peroxide of 30kg dicyclopentadiene, 28kg, the tungsten hexachloride of 0.4kg phenol modification and the glass fibre of 2kg are added in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 250 ℃ of left and right, continuing to add 1kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 3kg nano-calcium carbonate, 1kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 2mm is standby.
Preimpregnated glass fibre cloth: getting 2.6kg fineness is 350 object iron powders and tungsten powder mixture, then said mixture is mixed with 30kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 2kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 130 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 2 layers of unsaturated polyester sheet and 5 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 13mm left and right.
Embodiment 5
Prepare vibrin sheet: in temperature, be under 65 ℃ of conditions, by 45kg dicyclopentadiene, the hydrogen peroxide of 15kg, the glass fibre that the tungsten hexachloride of 0.4kg phenol modification and 1kg are woven into by glass fibre adds in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 250 ℃ of left and right, continuing to add 2kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 2kg nano-calcium carbonate, 2kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 1mm is standby.
Preimpregnated glass fibre cloth: getting 2.6kg fineness is 350 object iron powders and copper powder mixture, then said mixture is mixed with 38kg dicyclopentadiene unsaturated polyester, then add 2kg glasscloth to carry out preimpregnation, then in temperature, be to be dried in 130 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 7 layers of unsaturated polyester sheet and 8 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 13mm left and right.
Embodiment 6
Prepare vibrin sheet: in temperature, be under 50 ℃ of conditions, the hydrogen peroxide of 45kg dicyclopentadiene, 23kg, the tungsten hexachloride of 0.4kg phenol modification and the glass fibre of 1kg are added in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 250 ℃ of left and right, continuing to add 2kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 1kg nano silicon, 2kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 2mm is standby.
Preimpregnated glass fibre cloth: getting 2.6kg fineness is 350 object iron powders, copper powder and tungsten powder mixture, then said mixture is mixed with 20kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 3kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 130 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 6 layers of unsaturated polyester sheet and 6 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 20mm left and right.
Comparative example 1
Prepare vibrin sheet: in temperature, be under 50 ℃ of conditions, 55kg dicyclopentadiene, the tungsten hexachloride of 0.4kg phenol modification and the glass fibre of 4kg are added in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 250 ℃ of left and right, continuing to add 3kg brominated Polystyrene under the prerequisite stirring, its trade mark is PBS-64HW, 3kg nano silicon, 4kg potassium oxide, continue stirring reaction 6 left and right hour, can obtain resistant to elevated temperatures dicyclopentadiene unsaturated polyester resin.Then the unsaturated polyester resin sheet that this dicyclopentadiene unsaturated polyester is processed into 2mm is standby.
Preimpregnated glass fibre cloth: getting 2.6kg fineness is 350 object iron powders, copper powder and tungsten powder mixture, then said mixture is mixed with 25kg dicyclopentadiene unsaturated polyester, then add the glasscloth that 4kg is woven into by glass fibre to carry out preimpregnation, then in temperature, be to be dried in 130 ℃ of environment, obtain preimpregnated glass fibre cloth.
Prepare fiberglass reinforced plastic matrix material: respectively above-mentioned 6 layers of unsaturated polyester sheet and 6 layers of preimpregnated glass fibre cloth are prepared and formed high performance glass fiber reinforced plastics composite material by mould pressing process, the thickness of this glass fiber reinforced plastics composite material is 20mm left and right.
High temperature resistance polyester glass fiber reinforced plastics composite material of the present invention by adding hydrogen peroxide in dicyclopentadiene, can effectively improve softening temperature and the erosion resistance of fiberglass reinforced plastic matrix material, after potassium oxide adds, can react with water and generate potassium hydroxide, the effect with thickening also has fire-retardant effect simultaneously.By what add fiberglass reinforced plastic matrix material that Nano filling and glass fibre, metallic stuffing prepare, there is higher resistance to impact shock and flexural strength.
The method of preparing this high temperature resistance polyester glass fiber reinforced plastics composite material is to prepare by mould pressing process, 7 strata ester resin sheets and 9 layers of woven fiber glass cloth are dropped in mould, under more than 250 ℃ hot conditionss, utilize mold pressing that vibrin sheet and glasscloth can be merged preferably, prepare this fiberglass reinforced plastic matrix material, glass fibre is evenly distributed in material.
High temperature resistance polyester glass fiber reinforced plastics composite material of the present invention makes the dicyclopentadiene of part generate bicyclopentadiene dioxide by increasing hydrogen peroxide, therefore the fiberglass reinforced plastic matrix material being prepared into there is higher softening point temperature and the erosion resistance that has greatly improved this fiberglass reinforced plastic matrix material; In preparation, increase the glasscloth that glass fibre and glass fibre are made simultaneously, therefore improved greatly the bending strength of this fiberglass reinforced plastic matrix material; When preparing fiberglass reinforced plastic matrix material, add metal powder in addition, improved its shock resistance and wear resisting property.The performance of this high temperature resistance polyester glass fiber reinforced plastics composite material that referred to description that table 1 is detailed.
Table 1
The test condition of shore hardness is: according to standard GB/T/T230.2-2002, the shore hardness of fiberglass reinforced plastic matrix material is tested;
The test condition of flexural strength is: according to standard GB/T/T9341-2000, the flexural strength of fiberglass reinforced plastic matrix material is tested;
The test condition of resistance to impact shock is: according to standard GB/T/T9341-2008, the Izod otch resistance to impact shock of fiberglass reinforced plastic matrix material is tested;
The test condition of softening temperature is: according to standard GB/T/T5989-2008, the softening temperature of the firm matrix material of polyester glass is tested.
There is table 1 known, this fiberglass reinforced plastic matrix material has high strength, high corrosion resistance, the superperformance such as high temperature resistant and wear-resisting, can replace metal steel to prepare the various devices with particular requirement, as manufactured the fields such as space flight and aviation, automobile, anticorrosion, building body-building apparatus.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (7)
1. a glass fiber reinforced plastics composite material, it is characterized in that: the component by following weight percent forms: the tungsten hexachloride 0.1-0.5% of dicyclopentadiene 50-80%, hydrogen peroxide 10-30%, potassium oxide 1-3%, phenol modification, fire retardant 1-5%, Nano filling 2-4%, glass fibre 3-8%, metallic stuffing 1-3%, this glass fiber reinforced plastics composite material softening temperature is between 155-165 ℃, and its preparation mainly comprises the following steps:
Prepare resin sheet: in temperature, be under 30-60 ℃ of condition, by the dicyclopentadiene of 35-50% weight, the hydrogen peroxide of 10-30% weight, the tungsten hexachloride of the phenol modification of 0.1-0.5% weight and the glass fibre of 1-4% weight add in reactor, stir above-mentioned all substances are mixed, then the temperature of reactor is increased to 160-250 ℃, at the fire retardant that continues to add under the prerequisite stirring 1-5% weight, 2-4% weight Nano filling, 1-3% weight potassium oxide, continue stirring reaction 6-8 hour, obtain unsaturated polyester, then this resin treatment is become to unsaturated polyester sheet,
Preimpregnated glass fibre cloth: get the metallic stuffing of 1-3% weight and mix with 15-30% weight dicyclopentadiene unsaturated polyester, then add the glasscloth that 1-4% weight is woven into by glass fibre to carry out preimpregnation; After preimpregnation, glasscloth is carried out to drying treatment under 130-150 ℃ of environment, obtain preimpregnated glass fibre cloth;
Prepare glass fiber reinforced plastics composite material: some above-mentioned unsaturated polyester sheets and preimpregnated glass fibre cloth are prepared and formed glass fiber reinforced plastics composite material by mould pressing process.
2. glass fiber reinforced plastics composite material according to claim 1, is characterized in that: the weight percent of described hydrogen peroxide is 18-22% or 25-30%.
3. glass fiber reinforced plastics composite material according to claim 1, is characterized in that: described metallic stuffing is one or more in copper powder, iron powder or the tungsten powder of fineness between 200-500 order.
4. glass fiber reinforced plastics composite material according to claim 3, is characterized in that: the fineness of described metallic stuffing is 350 orders.
5. glass fiber reinforced plastics composite material according to claim 1, is characterized in that: described Nano filling is at least one in nano silicon or nano-calcium carbonate.
6. glass fiber reinforced plastics composite material according to claim 1, is characterized in that: the thickness of described glass fiber reinforced plastics composite material is 13-20mm.
7. glass fiber reinforced plastics composite material according to claim 1, is characterized in that: the shore hardness of described glass fiber reinforced plastics composite material is 98-108D, and flexural strength is 185-195MPa, and resistance to impact shock is 260
-285KJ/m
2.
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| CN101143919A (en) * | 2007-09-05 | 2008-03-19 | 中国科学院大连化学物理研究所 | Method for synthesizing alicyclic epoxy resin by catalyzing unsaturated alicyclic compound |
| CN101704823B (en) * | 2009-11-06 | 2011-09-14 | 四川东材科技集团股份有限公司 | Method for preparing bicyclopentadiene dioxide by catalysis through emulsion method |
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