CN104448793B - Plant fiber reinforced modified soy-based resin composite material - Google Patents
Plant fiber reinforced modified soy-based resin composite material Download PDFInfo
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Abstract
The invention discloses a plant fiber reinforced modified soy-based resin composite material and a preparation method thereof. Cross-linking agents and epoxidized soybean oil acrylate are blended to prepare soy-based resin, the soy-based resin is modified by modifiers to obtain modified soy-based resin, and plant fibers, the modified soy-based resin and initiators are hot-pressed to obtain the plant fiber reinforced modified soy-based resin composite material. The plant fiber reinforced modified soy-based resin composite material has excellent tensile strength, tensile modulus, bending strength, bending modulus and impact strength.
Description
Technical field
The invention belongs to natural plant fibre and strengthen resin composite materials technical field, be specifically related to a kind of Plant fiber's enhancing modified soybean oil based resin composite and preparation method thereof.
Background technology
Natural plant fibre strengthens in polymer composites, and the most frequently used thermosetting resin mainly has epoxy resin, phenolic resin and unsaturated polyester resin.Usually, these thermosetting resins have good mechanical property, chemical-resistance and processing performance, but environmental problem and air pollution problems inherent that in use the volatilization of noxious substance (such as formaldehyde, styrene etc.) is brought cause great concern.Additionally, constantly consuming of petroleum resources forces people to be sought for price rising problem and develops new reproducible bio-based resin.Epoxy soybean oil acrylate (Acrylate epoxidized
Soybean oil, i.e. AESO) it is to be obtained with acrylate reactions after epoxidation by soybean oil, produced the most in a large number, raw material sources are extensive, cheap, have been widely used in the field such as coating, degradable foamed material.Plant fiber/soybean oil based composites is prepared for raw material, owing to introducing of renewable Plant fiber and the oleoresinous use of plant are significant to the usage amount reducing petroleum-based products with AESO.But, the degree of cross linking is low, room temperature time viscosity is relatively big and the shortcoming such as poor heat resistance makes AESO must be blended with vinyl monomer in application process, be on the one hand to reduce resin viscosity, improve the preparation technology of composite；On the other hand, improve resin's crosslinkage, improve mechanical property and the heat resistance of composite.AESO is existing more report with the thermosetting resin of styrene copolymerized preparation good mechanical performance, but the use of volatile styrene still cannot avoid the problem of air pollution, and styrene is formally classified as carcinogen with sucking glass fibre by U.S. sanitaries in 2011 and public service administration.Therefore, seeking novel eco-friendly method and improve AESO cross-linkage of resin, the soybean oil based thermoset applications that processability is excellent is the key promoting AESO to be applied in natural fiber strengthens composite.In addition, the carboxylate of long-chain fatty acid is comprised on the molecular structure of AESO, containing 3 hydroxyls on its fatty acid, by introducing double-functional group monomer, AESO is modified, it is remarkably improved the degree of cross linking of soybean oil based resin, improves the mechanical property of Plant fiber/soybean oil based resin composite further.Use isophorone diisocyanate (IPDI) that soybean oil based resin is modified, with modified soybean oil based resin as matrix, be prepared for Plant fiber's enhancing modified soybean oil based resin composite.On the one hand, two NCOs of IPDI and the hydroxyl reaction of AESO can improve the crosslink density of resin, on the other hand, when two NCOs hydroxyl with fiber surface hydroxyl and AESO simultaneously of IPDI reacts, can improve the interface cohesion between fiber/resin, both of which can improve the mechanical property of composite.Therefore, the Plant fiber prepared by the present invention/modified soybean oil-based resin composite has excellent comprehensive mechanical property.
Summary of the invention
It is an object of the invention to provide a kind of Plant fiber's enhancing modified soybean oil based resin composite and preparation method thereof, solve petroleum base resin raw material sources short, expensive, the soybean oil based resin degree of cross linking is low, mechanical property is poor after solidification, the problem such as resin and interfibrous interface cohesion difference.Plant fiber/modified soybean oil-based resin the composite prepared has good hot strength, stretch modulus, bending strength, bending modulus and impact strength.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of Plant fiber's enhancing modified soybean oil based resin composite is to be prepared by hot press forming technology by the raw material of following parts by weight: Plant fiber 80 100 parts, modified soybean oil-based resin 80 100 parts, initiator 37 parts.
Described Plant fiber is hemp.
Described initiator is peroxidized t-butyl perbenzoate.
The oleoresinous preparation process of described modified soybean is: count by weight, magnetic agitation 5 10min after soybean oil based resin 80 95 parts and modifying agent 5 20 parts at room temperature being mixed, and i.e. obtains modified soybean oil-based resin；The preparation process of described soybean oil based resin is: count by weight, magnetic agitation 15 30min after soybean oil derivative 60 80 parts and cross-linking agent 20 40 parts at room temperature being mixed, and i.e. obtains soybean oil based resin；Described soybean oil derivative is epoxy soybean oil acrylate；Described cross-linking agent isN-vinyl pyrrolidone (N-vinyl-2-pyrrolidone, i.e. NVP)；Described modifying agent is isophorone diisocyanate (Isophorone diisocyanate, i.e. IPDI).
The method preparing Plant fiber's enhancing modified soybean oil based resin composite as above: will be coated in the upper and lower surface of Plant fiber's slab after modified soybean oil-based resin and initiator mix homogeneously, prepares described Plant fiber's enhancing modified soybean oil based resin composite by manual compression molding of mating formation.Specifically comprise the following steps that modified soybean oil-based resin and initiator mix and blend 0.5 2min, it is coated uniformly on the Plant fiber's slab (preparation method: dried Plant fiber is cooled to room temperature being dried, 59 fiber felt are arranged into fibre mat by orthogonal direction overlapping) upper and lower surface, at room temperature cold pressing 4 6min with 5 7MPa；Keep pressure constant, be warming up to 60 80 DEG C, pre-hot pressing 4 6min；It is continuously heating to 150 170 DEG C, hot pressing 20 40min；Heat insulation pressurize 30 90min, is allowed to naturally cool to room temperature.
The beneficial effects of the present invention is: the present invention uses the combination of process parameters of optimization, fiber and the oleoresinous amount ratio of modified soybean (mass ratio) are 1: 1, hot pressing temperature 160 DEG C, hot pressing time 30min, can prepare the Plant fiber/modified soybean oil-based resin composite of good mechanical performance with mould pressing process.Compared with Plant fiber/unmodified soybean oil based resin composite, Plant fiber's enhancing modified soybean oil based resin composite is used to have suitable impact strength and the hot strength, stretch modulus, bending strength and the bending modulus that significantly improve.
Accompanying drawing explanation
Fig. 1 is the tensile property of Plant fiber/modified soybean oil-based resin composite.Wherein, Control represents unmodified soybean oil based composites；IPDI-5 represents the soybean oil based composites using 5wt%IPDI modified；IPDI-10 represents the soybean oil based composites using 10wt%IPDI modified；IPDI-15 represents the soybean oil based composites using 15wt%IPDI modified；IPDI-20 represents the soybean oil based composites using 20wt%IPDI modified.In Fig. 2 with Fig. 3 abscissa, Control, IPDI-5, IPDI-10, IPDI-15 are identical with IPDI-20 implication.In figure, rectangular column upper and lower horizontal line represents the standard deviation of data mean value, and without significant difference between two groups of data mean values of expression of same letter above block diagram, otherwise difference is the most notable.
Fig. 2 is the bending property of Plant fiber/modified soybean oil-based resin composite.
Fig. 3 is the impact strength of Plant fiber/modified soybean oil-based resin composite.
Detailed description of the invention
Embodiment 1
Raw material: Plant fiber is hemp (hemp floss number is 130, and average length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited；Soybean oil based resin be byN-vinyl pyrrolidone (NVP) is blended with epoxy soybean oil acrylate (AESO) and obtains: NVP is purchased from Shanghai crystalline substance pure (Aladdin) Industrial Co., Ltd.；AESO(model: F03；Viscosity (23 DEG C): 8000 20000cps；Acid number :≤12 mgKOH/g) purchased from Jiangsu Litian Technology Co., Ltd.；Modifying agent is isophorone diisocyanate (IPDI), likes (Shanghai) chemical conversion industrial development company limited purchased from ladder is uncommon；Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Plant fiber/modified soybean oil-based resin composite:
The oleoresinous preparation process of modified soybean is: soybean oil based resin (95g) and modifying agent (5g) are placed in round-bottomed flask, with after magnetic stirrer 5 10min under room temperature, i.e. obtains modified soybean oil-based resin；Soybean oil based resin is the blend of AESO and NVP；Initiator is TBPB.
Composite material and preparation method thereof: weigh 75g modified soybean oil-based resin and 3.75g TBPB, stir evenly 1min with glass rod after mixing.When being cooled to room temperature after wrapping with plastic sealing bag after dried Plant fiber being taken out from baking oven, 59 fiber felt are arranged into fibre mat by orthogonal direction overlapping, the modified soybean oil-based resin mixed liquor even application of mix homogeneously on two surfaces of fibre mat, then move to cold pressing under room temperature and 6MPa pressure in punching block 5min, makes resin penetration enter in fibre mat.Then hot press is warming up to 70 DEG C of pre-hot pressing 5min under 6MPa；It is continuously heating to 160 DEG C, pressure 6MPa hot pressing 30min.Hot pressing completes rear mold heat insulation pressurize 60min, and is allowed to naturally cool to room temperature.
In described preparation process, soybean oil based resin and the amount ratio of modifying agent, be 19: 1 in mass ratio；Plant fiber and the oleoresinous amount ratio of modified soybean, be 1: 1 according to mass ratio；The consumption of initiator is the 5% of resin quality.
Embodiment 2
Raw material: Plant fiber is hemp (hemp floss number is 130, and average length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited；Soybean oil based resin be byN-vinyl pyrrolidone (NVP) is blended with epoxy soybean oil acrylate (AESO) and obtains: NVP is purchased from Shanghai crystalline substance pure (Aladdin) Industrial Co., Ltd.；AESO(model: F03；Viscosity (23 DEG C): 8000 20000cps；Acid number :≤12 mgKOH/g) purchased from Jiangsu Litian Technology Co., Ltd.；Modifying agent is isophorone diisocyanate (IPDI), likes (Shanghai) chemical conversion industrial development company limited purchased from ladder is uncommon；Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Plant fiber/modified soybean oil-based resin composite:
The oleoresinous preparation process of modified soybean is: soybean oil based resin (90g) and modifying agent (10g) are placed in round-bottomed flask, with after magnetic stirrer 5 10min under room temperature, i.e. obtains modified soybean oil-based resin；Soybean oil based resin is the blend of AESO and NVP；Initiator is TBPB.
Composite material and preparation method thereof: weigh 75g modified soybean oil-based resin and 3.75g TBPB, stir evenly 1min with glass rod after mixing.When being cooled to room temperature after wrapping with plastic sealing bag after dried Plant fiber being taken out from baking oven, 59 fiber felt are arranged into fibre mat by orthogonal direction overlapping, the modified soybean oil-based resin mixed liquor even application of mix homogeneously on two surfaces of fibre mat, then move to cold pressing under room temperature and 6MPa pressure in punching block 5min, makes resin penetration enter in fibre mat.Then hot press is warming up to 70 DEG C of pre-hot pressing 5min under 6MPa；It is continuously heating to 160 DEG C, pressure 6MPa hot pressing 30min.Hot pressing completes rear mold heat insulation pressurize 60min, and is allowed to naturally cool to room temperature.
In described preparation process, soybean oil based resin and the amount ratio of modifying agent, be 9: 1 in mass ratio；Plant fiber and the oleoresinous amount ratio of modified soybean, be 1: 1 according to mass ratio；The amount of initiator is the 5% of resin quality.
Embodiment 3
Raw material: Plant fiber is hemp (hemp floss number is 130, and average length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited；Soybean oil based resin be byN-vinyl pyrrolidone (NVP) is blended with epoxy soybean oil acrylate (AESO) and obtains: NVP is purchased from Shanghai crystalline substance pure (Aladdin) Industrial Co., Ltd.；AESO(model: F03；Viscosity (23 DEG C): 8000 20000cps；Acid number :≤12 mgKOH/g) purchased from Jiangsu Litian Technology Co., Ltd.；Modifying agent is isophorone diisocyanate (IPDI), likes (Shanghai) chemical conversion industrial development company limited purchased from ladder is uncommon；Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Plant fiber/modified soybean oil-based resin composite:
The oleoresinous preparation process of modified soybean is: soybean oil based resin (85g) and modifying agent (15g) are placed in round-bottomed flask, with after magnetic stirrer 5 10min under room temperature, i.e. obtains modified soybean oil-based resin；Soybean oil based resin is the blend of AESO and NVP；Initiator is TBPB.
Composite material and preparation method thereof: weigh 75g modified soybean oil-based resin and 3.75g TBPB, stir evenly 1min with glass rod after mixing.When being cooled to room temperature after wrapping with plastic sealing bag after dried Plant fiber being taken out from baking oven, 59 fiber felt are arranged into fibre mat by orthogonal direction overlapping, the modified soybean oil-based resin mixed liquor even application of mix homogeneously on two surfaces of fibre mat, then move to cold pressing under room temperature and 6MPa pressure in punching block 5min, makes resin penetration enter in fibre mat.Then hot press is warming up to 70 DEG C of pre-hot pressing 5min under 6MPa；It is continuously heating to 160 DEG C, pressure 6MPa hot pressing 30min.Hot pressing completes rear mold heat insulation pressurize 60min, and is allowed to naturally cool to room temperature.
In described preparation process, soybean oil based resin and the amount ratio of modifying agent, be 17: 3 in mass ratio；Plant fiber and the oleoresinous amount ratio of modified soybean, be 1: 1 according to mass ratio；The amount of initiator is the 5% of resin quality.
Embodiment 4
Raw material: Plant fiber is hemp (hemp floss number is 130, and average length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited；Soybean oil based resin be byN-vinyl pyrrolidone (NVP) is blended with epoxy soybean oil acrylate (AESO) and obtains: NVP is purchased from Shanghai crystalline substance pure (Aladdin) Industrial Co., Ltd.；AESO(model: F03；Viscosity (23 DEG C): 8000 20000cps；Acid number :≤12 mgKOH/g) purchased from Jiangsu Litian Technology Co., Ltd.；Modifying agent is isophorone diisocyanate (IPDI), likes (Shanghai) chemical conversion industrial development company limited purchased from ladder is uncommon；Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Plant fiber/modified soybean oil-based resin composite:
The oleoresinous preparation process of modified soybean is: soybean oil based resin (80g) and modifying agent (20g) are placed in round-bottomed flask, with after magnetic stirrer 5 10min under room temperature, i.e. obtains modified soybean oil-based resin；Soybean oil based resin is the blend of AESO and NVP；Initiator is TBPB.
Composite material and preparation method thereof: weigh 75g modified soybean oil-based resin and 3.75g TBPB, stir evenly 1min with glass rod after mixing.When being cooled to room temperature after wrapping with plastic sealing bag after dried Plant fiber being taken out from baking oven, 59 fiber felt are arranged into fibre mat by orthogonal direction overlapping, the modified soybean oil-based resin mixed liquor even application of mix homogeneously on two surfaces of fibre mat, then move to cold pressing under room temperature and 6MPa pressure in punching block 5min, makes resin penetration enter in fibre mat.Then hot press is warming up to 70 DEG C of pre-hot pressing 5min under 6MPa；It is continuously heating to 160 DEG C, pressure 6MPa hot pressing 30min.Hot pressing completes rear mold heat insulation pressurize 60min, and is allowed to naturally cool to room temperature.
In described preparation process, soybean oil based resin and the amount ratio of modifying agent, be 4: 1 in mass ratio；Plant fiber and the oleoresinous amount ratio of modified soybean, be 1: 1 according to mass ratio；The amount of initiator is the 5% of resin quality.
Composite panel Mechanics Performance Testing:
Composite panel makes dumbbell shape sample (specification: long 150mm, two ends width 20mm, middle wide 10mm, gauge length 106mm, thickness 3.0mm) to test tensile property；The test sample of bending property and impact strength is strip (specification: 80 mm × 10 mm × 3.0mm).Tensile property test is carried out according to GB1447-05 standard；Bending property test is carried out according to GB1449-05 standard；Impact strength test is according to GB/T1043-08.Tensile property and bending property test complete on microcomputer controlled electronic universal tester, and impact strength test completes on balance weight impact testing machine.
The hot strength of Plant fiber/modified soybean oil-based resin composite
Known by Fig. 1, compare with unmodified AESO based composites (hot strength is 61.56MPa), the composite hot strength of modifying agent IPDI consumption respectively 5%, 10%, 15% and 20% is 70.76MPa, 77.11MPa, 79.29MPa and 80.43MPa, has been respectively increased 14.94%, 25.26%, 28.80% and 30.65%.And, the hot strength of the composite that IPDI-10, IPDI-15 and IPDI-20 are modified is without significant difference.
The stretch modulus of Plant fiber/modified soybean oil-based resin composite
Known by Fig. 1, compare with unmodified AESO based composites (stretch modulus is 1945.92MPa), the composite tensile modulus of modifying agent IPDI consumption respectively 5%, 10%, 15% and 20% is 2108.64MPa, 2358.95MPa, 2441.55MPa and 2522.30MPa, has been respectively increased 8.36%, 21.23%, 25.47% and 29.62%.And, the stretch modulus of the composite that IPDI-10, IPDI-15 and IPDI-20 are modified is without significant difference.
The bending strength of Plant fiber/modified soybean oil-based resin composite
Known by Fig. 2, compare with unmodified AESO based composites (bending strength is 78.68MPa), the composite bending strength of modifying agent IPDI consumption respectively 5%, 10%, 15% and 20% is 94.26MPa, 107.74MPa, 112.37MPa and 118.10MPa, has been respectively increased 19.80%, 36.93%, 48.82% and 50.10%.And, the bending strength of the composite that IPDI-15 and IPDI-20 is modified is without significant difference.
The bending modulus of Plant fiber/modified soybean oil-based resin composite
Known by Fig. 2, unmodified AESO based composites (bending modulus is 5139.65MPa) compares, modifying agent IPDI consumption be 5%, 10%, 15% and 20% composite bending modulus be respectively 5954.61MPa, 6586.71MPa, 7014.72MPa and 7501.80MPa, be respectively increased 15.86%, 28.15%, 36.48% and 45.96%.And, the bending strength of the composite that IPDI-15 and IPDI-20 is modified is without significant difference.
The impact strength of Plant fiber/modified soybean oil-based resin composite
As seen from Figure 3, the interpolation of modifying agent does not significantly change the impact strength of Plant fiber/modified soybean oil-based resin composite, and unmodified AESO base resin, the composite impact intensity of the AESO base resin adding 5%, 10%, 15% and 20%IPDI are respectively 22.35 kJ/m2、22.11
kJ/m2、22.62 kJ/m2、22.85kJ/m2And 20.25kJ/m2。
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.
Claims (5)
1. Plant fiber's enhancing modified soybean oil based resin composite, it is characterised in that: described composite is to be prepared by hot press forming technology by the raw material of following parts by weight: Plant fiber 80 100 parts, modified soybean oil-based resin 80 100 parts, initiator 37 parts；The oleoresinous preparation process of described modified soybean is: count by weight, magnetic agitation 5 10min after soybean oil based resin 80 95 parts and modifying agent 5 20 parts at room temperature being mixed, and i.e. obtains modified soybean oil-based resin；The preparation process of described soybean oil based resin is: count by weight, magnetic agitation 15 30min after soybean oil derivative 60 80 parts and cross-linking agent 20 40 parts at room temperature being mixed, and i.e. obtains soybean oil based resin；Described soybean oil derivative is epoxy soybean oil acrylate；Described cross-linking agent isN-vinyl pyrrolidone；Described modifying agent is isophorone diisocyanate.
Plant fiber's enhancing modified soybean oil based resin composite the most according to claim 1, it is characterised in that: described Plant fiber is hemp.
Plant fiber's enhancing modified soybean oil based resin composite the most according to claim 1, it is characterised in that: described initiator is peroxidized t-butyl perbenzoate.
4. the method preparing Plant fiber's enhancing modified soybean oil based resin composite as claimed in claim 1, it is characterized in that: the upper and lower surface of Plant fiber's slab will be coated in after modified soybean oil-based resin and initiator mix homogeneously, prepare described Plant fiber's enhancing modified soybean oil based resin composite by manual compression molding of mating formation.
Method the most according to claim 4, it is characterized in that: specifically comprise the following steps that modified soybean oil-based resin and initiator mix and blend 0.5 2min, it is coated uniformly on the upper and lower surface of Plant fiber's slab being dried, at room temperature colds pressing 4 6min with 5 7MPa；Keep pressure constant, be warming up to 60 80 DEG C, pre-hot pressing 4 6min；It is continuously heating to 150 170 DEG C, hot pressing 20 40min；Heat insulation pressurize 30 90min, is allowed to naturally cool to room temperature.
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| CN104788733B (en) * | 2015-04-18 | 2016-10-05 | 福建农林大学 | A kind of isocyanate-crosslinked soybean oil based resin/natural-fiber composite material |
| CN104786314B (en) * | 2015-04-18 | 2016-08-17 | 福建农林大学 | Soybean oil based resin/fibrous composite that a kind of acrylic acid is isocyanate-crosslinked |
| CN106750553B (en) * | 2017-03-02 | 2019-05-31 | 华南理工大学 | Biodegradable composite material and preparation method and application |
| CN108084667B (en) * | 2018-01-16 | 2019-10-22 | 福建农林大学 | A kind of modified microcrystalline cellulose enhancing soybean oil based resin composite material and preparation method |
| CN110938285A (en) * | 2018-09-21 | 2020-03-31 | 广西大学 | Bagasse and glass fiber composite reinforced epoxy resin material and preparation method thereof |
| CN112266575B (en) * | 2020-10-29 | 2022-11-01 | 咸阳新伟华绝缘材料有限公司 | High-temperature-resistant epoxy resin encapsulating material and preparation method thereof |
| CN116535138B (en) * | 2023-05-04 | 2024-05-10 | 广东水电二局股份有限公司 | Asphalt concrete and preparation method and application thereof |
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| CN101289570B (en) * | 2008-03-18 | 2011-01-12 | 中山大学 | Epoxy soybean oil resin based rigid cellular plastic and method for preparing same |
| CN103980438B (en) * | 2014-01-22 | 2016-08-17 | 湖北大学 | The preparation of ultraviolet curing type soybean oil base compound resin |
| CN104212142B (en) * | 2014-09-18 | 2016-04-06 | 福建农林大学 | The plant oil based unsaturated polyester composite of a kind of bamboo fiber enhancing modified |
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