CN104448846B - Plant fiber reinforced soy-based resin composite material and preparation method thereof - Google Patents
Plant fiber reinforced soy-based resin composite material and preparation method thereof Download PDFInfo
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- CN104448846B CN104448846B CN201410839591.1A CN201410839591A CN104448846B CN 104448846 B CN104448846 B CN 104448846B CN 201410839591 A CN201410839591 A CN 201410839591A CN 104448846 B CN104448846 B CN 104448846B
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Abstract
The invention discloses a plant fiber reinforced 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, and plant fibers, the soy-based resin and initiators are hot-pressed to obtain the plant fiber reinforced soy-based resin composite material. The plant fiber reinforced 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 reinforced resin technical field of composite materials, and in particular to a kind of string increases
Powerful 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, phenol
Urea formaldehyde and unsaturated polyester resin.Usually, these thermosetting resins have good mechanical property, chemical-resistance and work
Skill performance, but noxious material in use（Such as formaldehyde, styrene）The environmental problem brought of volatilization and air it is dirty
Dye problem causes great concern.Additionally, the continuous consumption of petroleum resources and price rise problem force people to be sought for and
The new reproducible bio-based resin of exploitation.Epoxy soybean oil acrylate（Acrylate epoxidized soybean
Oil, i.e. AESO）It is to be obtained with propylene acid reaction Jing after epoxidation by soybean oil, has commercially been produced in a large number at present, it is former
Material wide material sources, cheap, have been widely used in the fields such as coating, degradable foamed material.Prepare by raw material of AESO
String/soybean oil based composites, because the introducing and the oleoresinous use of plant of renewable string is to reducing
The usage amount of petroleum-based products is significant.However, the degree of cross linking is low, normal temperature when viscosity is larger and causes the shortcomings of poor heat resistance
AESO must be blended in application process with vinyl monomer, on the one hand be to reduce resin viscosity, improve composite
Preparation technology；On the other hand, resin crosslink density can be improved, improves the mechanical property and heat resistance of composite.AESO
With the existing more report of thermosetting resin of styrene copolymerized preparation good mechanical performance, but the use of volatile styrene still without
Method avoids the problem of air pollution, and U.S. sanitaries in 2011 and public service from affixing one's name to formally by styrene and inhalable glass
Fiber is classified as carcinogenic substance.Therefore, seek the high solvent of new eco-friendly reactivity and prepare soybean oil with AESO blendings
Based thermoset applications are to promote AESO to strengthen the key being applied in composite in natural fiber.Additionally, with AESO as base
Body prepares composite material of plant fiber, and the carboxylate comprising LCFA, on its aliphatic acid 3 are contained on the molecular structure of AESO
Individual hydroxyl, by the hydrogen bond action with fiber surface hydroxyl, shows and the preferable compatibility of string, can prepare comprehensive
String/soybean oil based resin the composite of better performances is learned with joint efforts.
The content of the invention
It is an object of the invention to provide a kind of string strengthens soybean oil based resin composite and preparation method thereof,
Solve petroleum base resin raw material sources short, expensive, environmental pollution etc. caused by noxious material release institute in preparation process
Problem.Obtained string strengthens soybean oil based resin composite and has good tensile strength, stretch modulus, bending strong
Degree, bending modulus and impact strength.
For achieving the above object, the present invention is adopted the following technical scheme that：
It is by being hot pressed into by the raw material of following parts by weight that a kind of string strengthens soybean oil based resin composite
Obtained in type technique：80-100 parts of string, 80-100 parts of soybean oil based resin, 3-7 parts of initiator.
Described string is hemp.
Described initiator is peroxidized t-butyl perbenzoate.
The preparation process of described soybean oil based resin is：Count by weight, by 60-80 parts of soybean oil derivative and friendship
Join-the 30min of magnetic agitation 15 after 20-40 parts of agent mixes at room temperature, that is, obtain soybean oil based resin；Described soybean oil derives
Thing is epoxy soybean oil acrylate；Described crosslinking agent isN- vinyl pyrrolidone（N- vinyl-2-pyrrolidone,
That is NVP）.
Prepare the method that string as above strengthens soybean oil based resin composite：By soybean oil based resin and
Initiator is coated in the upper and lower surface of string slab after being well mixed, described plant is obtained by manual compression molding of mating formation
Fibres strengthen soybean oil based resin composite.Comprise the following steps that：Soybean oil based resin and initiator are mixed
0.5-2min, is coated uniformly on dry string slab（Preparation method：Dried string is cooled to into room
Temperature, 5-9 fibrofelts are arranged into fibre mat by orthogonal direction overlapping）Upper and lower surface, cold pressing 4 with 5-7MPa under room temperature-
6min；Keep pressure constant, be warming up to 60-80 DEG C ,-the 6min of pre- hot pressing 4；It is continuously heating to 150-170 DEG C, hot pressing 20-
40min；- the 90min of heat-insulated pressurize 30, is allowed to naturally cool to room temperature.
The beneficial effects of the present invention is：The present invention is using the combination of process parameters for optimizing, fiber and soybean oil based resin
Amount ratio（Mass ratio）For 1: 1,160 DEG C of hot pressing temperature, hot pressing time 30min can prepare mechanical property excellent with mould pressing process
Good string/soybean oil based resin composite.Compared with string/pure AESO resin composite materials, using NVP with
String based on AESO blends/soybean oil based resin composite has suitable impact strength and significantly improves
Tensile strength, stretch modulus, bending strength and bending modulus.
Description of the drawings
Fig. 1 is the tensile property of string/soybean oil based resin composite.Wherein, AESO is represented using pure AESO
Composite based on resin；30St represents the composite for adopting 30wt% styrene for AESO crosslinking agents；20NVP is represented
Adopt 20wt%NVP for AESO crosslinking agents composite；30NVP represents the composite wood for adopting 30wt%NVP for AESO crosslinking agents
Material；40NVP represents the composite for adopting 40wt%NVP for AESO crosslinking agents；AESO in Fig. 2 and Fig. 3 abscissas, 30St,
20NVP, 30NVP are identical with 40NVP implications.Rectangular column upper and lower horizontal line represents the standard deviation of data mean value in figure, on block diagram
Significant difference between the two groups of data mean values of expression of side without same letter, otherwise difference is not notable.
Fig. 2 is the bending property of string/soybean oil based resin composite.
Fig. 3 is the impact strength of string/soybean oil based resin composite.
Specific embodiment
Embodiment 1
Raw material：String is hemp（Hemp suede number is 130, and average length is 3cm）, purchased from Anhui copper
Mound Samsung Ma Ye Co., Ltds；Soybean oil derivative is epoxy soybean oil acrylate（AESO）（Model：F03；Viscosity (23
℃)：8000–20000cps；Acid number：≤ 12 mgKOH/g）, purchased from Jiangsu Litian Technology Co., Ltd.；Crosslinking agent isN-
Vinyl pyrrolidone（NVP）, it is pure purchased from Shanghai crystalline substance（Aladdin）Industrial Co., Ltd.；Initiator is the tertiary fourth of perbenzoic acid
Ester（TBPB）, purchased from Sigma-Aldrich（Shanghai）Trade Co., Ltd.
String/soybean oil based resin composite：
The preparation process of soybean oil based resin is：By soybean oil derivative（80g）And crosslinking agent（20g）It is placed in round-bottomed flask
In, with after-the 30min of magnetic stirrer 15 under room temperature, that is, obtain soybean oil based resin mixed liquor；Soybean oil derivative is
AESO；Crosslinking agent is NVP；Initiator is TBPB.
Composite material and preparation method thereof：75g soybean oil based resins mixed liquor and 3.75g TBPB are weighed, is stirred with glass rod after mixing
Even 1min.When being cooled to room temperature after being wrapped with plastic sealing bag after dried string is taken out from baking oven, 5-9
Fibrofelt is arranged into fibre mat by orthogonal direction overlapping, and the soybean oil based resin and additive even application that are well mixed are existed
Two surfaces of fibre mat, then move in punching block the 5min that colds pressing under room temperature and 6MPa pressure, make resin penetration enter fiber
In slab.Then hot press is warming up to 70 DEG C of pre- hot pressing 5min under 6MPa；160 DEG C are continuously heating to, pressure 6MPa hot pressing
30min.Mould heat insulation pressurize 60min after the completion of hot pressing, and be allowed to naturally cool to room temperature.
In the preparation process, the amount ratio of soybean oil derivative and crosslinking agent, is in mass ratio 4: 1；String with
The amount ratio of soybean oil based resin mixed liquor, is 1: 1 according to mass ratio；The consumption of initiator is the 5% of resin quality.
Embodiment 2
Raw material：String is hemp（Hemp suede number is 130, and average length is 3cm）, purchased from Anhui copper
Mound Samsung Ma Ye Co., Ltds；Soybean oil derivative is epoxy soybean oil acrylate（AESO）（Model：F03；Viscosity (23
℃)：8000–20000cps；Acid number：≤ 12 mgKOH/g）, purchased from Jiangsu Litian Technology Co., Ltd.；Crosslinking agent isN-
Vinyl pyrrolidone（NVP）, it is pure purchased from Shanghai crystalline substance（Aladdin）Industrial Co., Ltd.；Initiator is the tertiary fourth of perbenzoic acid
Ester（TBPB）, purchased from Sigma-Aldrich（Shanghai）Trade Co., Ltd.
String/soybean oil based resin composite：
The preparation process of soybean oil based resin is：By soybean oil derivative（70g）And crosslinking agent（30g）It is placed in round-bottomed flask
In, with after 15 ~ 30min of magnetic stirrer under room temperature, that is, obtain soybean oil based resin mixed liquor；Soybean oil derivative is
AESO；Crosslinking agent is NVP；Initiator is TBPB.
Composite material and preparation method thereof：75g soybean oil based resins mixed liquor and 3.75g TBPB are weighed, is stirred with glass rod after mixing
Even 1min.When being cooled to room temperature after being wrapped with plastic sealing bag after dried string is taken out from baking oven, 5-9
Fibrofelt is arranged into fibre mat by orthogonal direction overlapping, and the soybean oil based resin and additive even application that are well mixed are existed
Two surfaces of fibre mat, then move in punching block the 5min that colds pressing under room temperature and 6MPa pressure, make resin penetration enter fiber
In slab.Then hot press is warming up to 70 DEG C of pre- hot pressing 5min under 6MPa；160 DEG C are continuously heating to, pressure 6MPa hot pressing
30min.Mould heat insulation pressurize 60min after the completion of hot pressing, and be allowed to naturally cool to room temperature.
In the preparation process, the amount ratio of soybean oil derivative and crosslinking agent, is in mass ratio 7: 3；String with
The amount ratio of soybean oil based resin mixed liquor, is 1: 1 according to mass ratio；The consumption of initiator is the 5% of resin quality.
Embodiment 3
Raw material：String is hemp（Hemp suede number is 130, and average length is 3cm）, purchased from Anhui copper
Mound Samsung Ma Ye Co., Ltds；Soybean oil derivative is epoxy soybean oil acrylate（AESO）（Model：F03；Viscosity (23
℃)：8000–20000cps；Acid number：≤ 12 mgKOH/g）, purchased from Jiangsu Litian Technology Co., Ltd.；Crosslinking agent isN-
Vinyl pyrrolidone（NVP）, it is pure purchased from Shanghai crystalline substance（Aladdin）Industrial Co., Ltd.；Initiator is the tertiary fourth of perbenzoic acid
Ester（TBPB）, purchased from Sigma-Aldrich（Shanghai）Trade Co., Ltd.
String/soybean oil based resin composite：
The preparation process of soybean oil based resin is：By soybean oil derivative（60g）And crosslinking agent（40g）It is placed in round-bottomed flask
In, with after-the 30min of magnetic stirrer 15 under room temperature, that is, obtain soybean oil based resin mixed liquor；Soybean oil derivative is
AESO；Crosslinking agent is NVP；Initiator is TBPB.
Composite material and preparation method thereof：75g soybean oil based resins mixed liquor and 3.75g TBPB are weighed, is stirred with glass rod after mixing
Even 1min.When being cooled to room temperature after being wrapped with plastic sealing bag after dried string is taken out from baking oven, 5-9
Fibrofelt is arranged into fibre mat by orthogonal direction overlapping, and the soybean oil based resin and additive even application that are well mixed are existed
Two surfaces of fibre mat, then move in punching block the 5min that colds pressing under room temperature and 6MPa pressure, make resin penetration enter fiber
In slab.Then hot press is warming up to 70 DEG C of pre- hot pressing 5min under 6MPa；160 DEG C are continuously heating to, pressure 6MPa hot pressing
30min.Mould heat insulation pressurize 60min after the completion of hot pressing, and be allowed to naturally cool to room temperature.
In the preparation process, the amount ratio of soybean oil derivative and crosslinking agent, is in mass ratio 3: 2；String with
The amount ratio of soybean oil based resin mixed liquor, is 1: 1 according to mass ratio；The consumption 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 width 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 standards；Bending property test is according to GB1449-05
Standard is carried out；Impact strength test is according to GB/T1043-08.Tensile property and bending property test are omnipotent in microcomputer controlled electronic
Complete on testing machine, impact strength test is completed on balance weight impact testing machine.
The tensile strength of string/soybean oil based resin composite
Known by Fig. 1, with pure AESO based composites（Tensile strength is 49.46MPa）Relatively, crosslinking agent NVP consumptions difference
Composite tensile strength for 20wt%, 30wt% and 40wt% is 60.65MPa, 67.66MPa and 82.57MPa, is respectively increased
22.62%, 36.80% and 66.94%.And, the tensile strength of 20NVP and 30NVP composites and 30% styrene composite wood
The tensile strength of material（64.12MPa）Without significant difference, but 40NVP composites then significantly improve 29.64%.
The stretch modulus of string/soybean oil based resin composite
Known by Fig. 1, with pure AESO based composites（Stretch modulus is 1690.69MPa）Relatively, crosslinking agent NVP consumptions point
Not Wei 20wt%, 30wt% and 40wt% composite tensile modulus be 2080.96MPa, 2217.37MPa and 2612.30MPa,
It has been respectively increased 23.08%, 31.15% and 54.51%.And, the stretch modulus of 20NVP and 30NVP composites and 30% benzene second
The stretch modulus of alkene composite（2134.57MPa）Without significant difference, but 40NVP composites then significantly improve 22.38%.
The bending strength of string/soybean oil based resin composite
Known by Fig. 2, with pure AESO based composites（Bending strength is 56.67MPa）Relatively, crosslinking agent NVP consumptions difference
Composite bending strength for 20wt%, 30wt% and 40wt% is 83.46MPa, 90.59MPa and 100.93MPa, is respectively increased
47.27%, 59.86% and 78.10%.And, the bending of the bending strength of 20NVP composites and 30% benzene composite material
Intensity（82.40MPa）Without significant difference, but 30NVP and 40NVP composites then significantly improve respectively 9.94% and 22.49%.
The bending modulus of string/soybean oil based resin composite
Known by Fig. 2, with pure AESO based composites（Bending modulus is 3799.19MPa）Relatively, crosslinking agent NVP consumptions point
Not Wei 20wt%, 30wt% and 40wt% composite bending modulus be 5423.47MPa, 6065.31MPa and 6717.44MPa,
It has been respectively increased 42.75%, 59.65% and 76.81%.And, the bending modulus of 20NVP composites and 30% styrene composite wood
The bending modulus of material（5570.88MPa）Without significant difference, but 30NVP and 40NVP composites are then respectively increased 8.88% He
20.58%。
The impact strength of string/soybean oil based resin composite
Known by Fig. 3, the addition of crosslinking agent does not significantly change the impact of string/soybean oil based resin composite
Intensity, pure AESO bases resin, the composite impact of addition 20wt%St, 20wt%NVP, 30wt%NVP and 40wt%NVP crosslinking agent
Intensity is respectively 22.806 kJ/m2、24.120 kJ/m2、25.344 kJ/m2、23.658 kJ/m2With 22.762 kJ/m2。
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (1)
1. a kind of string strengthens the preparation method of soybean oil based resin composite, it is characterised in that：
The preparation process of soybean oil based resin is：Soybean oil derivative 60g and crosslinking agent 40g are placed in round-bottomed flask, room temperature
After the lower -30min of use magnetic stirrer 15, that is, obtain soybean oil based resin mixed liquor；Soybean oil derivative is AESO；Hand over
Connection agent is NVP；Initiator is TBPB；
Composite material and preparation method thereof：75g soybean oil based resins mixed liquor and 3.75g TBPB are weighed, is stirred evenly with glass rod after mixing
1min, when being cooled to room temperature after being wrapped with plastic sealing bag after dried string is taken out from baking oven, 5-9
Fibrofelt is arranged into fibre mat by orthogonal direction overlapping, and the soybean oil based resin and additive even application that are well mixed are existed
Two surfaces of fibre mat, then move in punching block the 5min that colds pressing under room temperature and 6MPa pressure, make resin penetration enter fiber
In slab, then hot press is warming up to 70 DEG C of pre- hot pressing 5min under 6MPa；160 DEG C are continuously heating to, pressure 6MPa hot pressing
30min, mould heat insulation pressurize 60min after the completion of hot pressing, and be allowed to naturally cool to room temperature；
In the preparation process, the amount ratio of soybean oil derivative and crosslinking agent, is in mass ratio 3: 2；String with it is big
The amount ratio of soybean oil based resin mixed liquor, is 1: 1 according to mass ratio；The consumption of initiator is the 5% of resin quality.
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| CN108264731A (en) * | 2017-01-19 | 2018-07-10 | 宁波华翔自然纤维科技有限公司 | Plant fiber felt ring (collar O compoiste material and its preparation method and application |
| CN108264774A (en) * | 2017-01-19 | 2018-07-10 | 宁波华翔自然纤维科技有限公司 | A kind of composite honeycomb battenboard and its manufacturing method |
| CN107858009A (en) * | 2017-11-21 | 2018-03-30 | 福建农林大学 | A kind of string enhancing methacrylate soybean oil based resin composite and preparation method thereof |
| 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 |
| 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 |
| CN115160982B (en) * | 2022-08-09 | 2023-08-04 | 福建农林大学 | Preparation method and application of waterproof soybean oil-based wood adhesive |
| 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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| CN1294189C (en) * | 2005-03-03 | 2007-01-10 | 北京化工大学 | Reaction liquid for modifying polymer film and modifying method |
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| CN101289570A (en) * | 2008-03-18 | 2008-10-22 | 中山大学 | Epoxy soybean oil resin based rigid cellular plastic and method for preparing same |
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