CN104628966A - Plant fiber reinforced environment-friendly unsaturated polyester composite material - Google Patents
Plant fiber reinforced environment-friendly unsaturated polyester composite material Download PDFInfo
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- CN104628966A CN104628966A CN201510034264.3A CN201510034264A CN104628966A CN 104628966 A CN104628966 A CN 104628966A CN 201510034264 A CN201510034264 A CN 201510034264A CN 104628966 A CN104628966 A CN 104628966A
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Abstract
The invention discloses a plant fiber reinforced environment-friendly unsaturated polyester composite material and a preparation method thereof. The composite material is prepared through taking tri(ethylene glycol) divinyl ether as a reactive solvent of solid unsaturated polyester and taking plant fibers as a reinforcement. The plant fiber reinforced environment-friendly unsaturated polyester composite material is prepared from the plant fibers, the reactive solvent, solid styrene-free unsaturated polyester and an initiator through hot-press molding. According to the composite material prepared by the preparation method, the used environment-friendly unsaturated polyester does not contain a carcinogenic reactive solvent, namely styrene, and has the characteristics of environment-friendliness and low cost; the prepared composite material has very high tensile strength, flexural strength, flexural 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 vegetable fibre and strengthen environmentally friendly unsaturated polyester composite and preparation method thereof.
Background technology
In recent years, the research utilizing natural plant fibre to strengthen polymer composites receives extensive concern.Hemp fibre has that output is large, distribution is wide, intensity and modulus advantages of higher, is a kind of strongthener with broad prospect of application.Unsaturated polyester (UPE) is the resin variety that in galss fiber reinforced resin matrix material, consumption is maximum.UPE resin mechanical property and manufacturability well, but use volatile vinylbenzene as thinner and linking agent in preparation process in a large number, and the air pollution problems inherent brought thus causes great concern.U.S. sanitaries in 2011 and public service administration formally by vinylbenzene with can suck glass fibre and be classified as carcinogens.Therefore, for fiber-reinforced resin matrix compound material industry, new reinforcement must be sought to reduce glass fibre usage quantity as far as possible, take measures to reduce the vinylbenzene consumption in matrix material preparation simultaneously.Current research in this regard both at home and abroad mainly contains: one is adopt polyurethane, trimeric cyanamide, resol etc. and UPE resin alloy, and to reduce vinylbenzene usage quantity and burst size, but the resin viscosity of preparation is high, and cost increases, complicated process of preparation; Two is in UPE resin, add functional vegetable and animals oils reduce cinnamic usage quantity, modification vegetable and animals oils is by synthesizing new resins such as radical polymerization, cationoid polymerisation, ring-opening metathesis polymerizations, but building-up process is still using Vinyl toluene or Dicyclopentadiene (DCPD) etc. as linking agent and thinner, the toxicity such as Vinyl toluene are larger, and this resinoid mechanical property is lower; Three is the reactive solvents using acrylic ester monomer as UPE resin, but resin wetting property is low, viscosity is large, glass transition temperature is low with solidification rate, and composite materials property is deteriorated.Be that UPE resin prepared by raw material with vegetable and animals oils, significant to the usage quantity reducing petroleum-based products, but generally must add some petroleum-based mixtures to obtain good performance, these material composition thermostabilitys are poor and lack and participate in some active groups of resin solidification.Therefore, not yet have at present not containing the basic solution of cinnamic novel UPE process for preparing resins.
Summary of the invention
The object of the present invention is to provide a kind of vegetable fibre to strengthen environmentally friendly UPE matrix material and preparation method thereof, solve vinylbenzene usage quantity in traditional UPE resin large, cause the problems such as atmospheric pollution.Vegetable fibre prepared by the present invention strengthens environmentally friendly UPE matrix material and has very high tensile strength, flexural strength, modulus in flexure and shock strength.
For achieving the above object, the present invention adopts following technical scheme:
It is obtained by hot press forming technology by vegetable fibre, environmentally friendly UPE resin and initiator that a kind of vegetable fibre strengthens environmentally friendly UPE matrix material; Described vegetable fibre is hemp fibre; Described environmentally friendly UPE resin adopts reactive solvents and solid UPE is blended obtains under certain condition; Described initiator is peroxidized t-butyl perbenzoate.
The mass fraction of described matrix material feed composition is: 80 ~ 100 parts, vegetable fibre, environmentally friendly UPE resin 80 ~ 100 parts; Initiator 3 ~ 7 parts.
The preparation process of described environmentally friendly UPE resin is: solid UPE 40 ~ 60 parts and reactive solvents 40 ~ 60 parts are mixed to get environmentally friendly UPE resin under certain condition; Described solid UPE is m-phthalic acid type unsaturated polyester; Described reactive solvents is triethyleneglycol divinylether (English by name: Tri (ethylene glycol) divinyl ether, i.e. TDE).
The concrete preparation process that a kind of vegetable fibre as above strengthens environmentally friendly UPE matrix material is as follows:
(1) vegetable fibre after being cut into 20 cm × 20 cm fibrefelts, is dried to over dry at being placed in 100 ~ 105 DEG C through shredding;
(2) solid is ground to 80 ~ 100 order powder without vinylbenzene UPE 40 ~ 60 parts for subsequent use; Reactive solvents 40 ~ 60 parts is placed in after flask heats under 75 DEG C of water-baths, slowly adds solid and dissolves completely to it without magnetic agitation after vinylbenzene unsaturated polyester powder; Taking-up is cooled to room temperature, namely obtains environmentally friendly UPE resin;
(3) take the environmentally friendly UPE resin 80 ~ 100 parts of step (2) and initiator 3 ~ 7 parts of mix and blend 2min, obtain environmentally friendly UPE resin mixture liquor; The vegetable fibre felt of 5 ~ 9 steps (1) is arranged into fibre mat by orthogonal directions is superimposed, two surfaces of rapid for resin mixture liquor even application in fibre mat, then to move in punching block and to cold pressing 4 ~ 6min with the pressure of 5 ~ 7MPa at 70 DEG C, make resin penetration enter in fibre mat; Then thermocompressor is warming up to 150 ~ 170 DEG C of hot pressing 20 ~ 40min under 5 ~ 7MPa pressure; Hot pressing completes the heat insulation pressurize 30 ~ 90min of rear mold, makes it to naturally cool to room temperature.
Beneficial effect of the present invention is: the present invention adopts the combination of process parameters of optimization, the amount ratio (mass ratio) of vegetable fibre and environmentally friendly UPE resin is 1: 1, hot pressing temperature 160 DEG C, hot pressing time 30min, the vegetable fibre can preparing good mechanical performance with mould pressing process strengthens environmentally friendly UPE matrix material.Adopt environmentally friendly UPE as the matrix of matrix material, gained matrix material and traditional UPE resin (taking vinylbenzene as solvent) have suitable tensile strength for the matrix material of matrix, slightly low flexural strength and modulus in flexure, but there is higher shock strength.
Accompanying drawing explanation
Fig. 1 is the tensile strength of vegetable fibre/environmentally friendly UPE matrix material.Wherein, St-40 represents that employing 40wt% vinylbenzene is the matrix material of UPE solvent; TDE-40 represents that employing 40wt%TDE is the matrix material of UPE solvent; TDE-50 represents that employing 50wt%TDE is the matrix material of UPE solvent; In Fig. 2 with Fig. 3 X-coordinate, St-40, TDE-40 and TDE-50 represent that implication is identical.In figure, rectangular column upper and lower horizontal line represents the standard deviation of data mean value, and without significant difference between expression two groups of data of same letter above histogram, otherwise difference is not remarkable.
Fig. 2 is the bending property of vegetable fibre/environmentally friendly matrix material.
Fig. 3 is the shock strength of vegetable fibre/environmentally friendly matrix material.
Embodiment
Embodiment 1
Raw material: vegetable fibre is hemp fibre (hemp fibre suede number is 130, and mean length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited; Solid is m-phthalic acid type unsaturated polyester without vinylbenzene unsaturated polyester (UPE), is synthesized and obtains: propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE equal purchased from American Sigma-Aldrich company by propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE; Reactive solvents is triethyleneglycol divinylether (TDE), purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Vegetable fibre strengthens environmentally friendly UPE matrix material:
Environmentally friendly UPE resin is obtained than blended solid without vinylbenzene UPE and reactive solvents by certain quality.Vegetable fibre, environmentally friendly UPE resin and initiator are strengthened environmentally friendly UPE matrix material by the hot-forming vegetable fibre that obtains.Reactive solvents is TDE, and the preparation process of environmentally friendly UPE resin is: solid is ground to 80 ~ 100 order powder without vinylbenzene UPE 60g for subsequent use; Reactive solvents TDE 40g is placed in after flask heats under 75 DEG C of water-baths, slowly adds solid and dissolves completely to it without magnetic agitation after vinylbenzene UPE powder; Taking-up is cooled to room temperature, namely obtains environmentally friendly UPE resin; The solid adopted is m-phthalic acid type UPE without vinylbenzene UPE, is synthesized obtain by propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE.
Composite material and preparation method thereof: vegetable fibre is through shredding and after being cut into 20 cm × 20 cm fibrefelts, be dried to over dry at being placed in 100 ~ 105 DEG C; Take environmentally friendly UPE resin 75 g and initiator 3.75 g mix and blend 2min, obtain environmentally friendly UPE resin mixture liquor; By 5 ~ 9 vegetable fibre felts, (75 g) are arranged into fibre mat by orthogonal directions is superimposed, two surfaces of rapid for resin mixture liquor even application in fibre mat, then to move in punching block and to cold pressing 5min with the pressure of 6MPa at 70 DEG C, make resin penetration enter in fibre mat; Then thermocompressor is warming up to 160 DEG C of hot pressing 30min under 6MPa pressure; Hot pressing completes the heat insulation pressurize 60min of rear mold, makes it to naturally cool to room temperature.
In described preparation process, reactive solvents and solid, without the amount ratio of vinylbenzene UPE, are 2:3 according to mass ratio; The amount ratio 1: 1 of vegetable fibre and environmentally friendly UPE resin; The consumption of initiator is 5% of environmentally friendly UPE resin quality.
Embodiment 2
Raw material: vegetable fibre is hemp fibre (hemp fibre suede number is 130, and mean length is 3cm), purchased from Tongling, Anhui Province Samsung Ma Ye company limited; Solid is m-phthalic acid type unsaturated polyester without vinylbenzene unsaturated polyester (UPE), is synthesized and obtains: propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE equal purchased from American Sigma-Aldrich company by propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE; Reactive solvents is triethyleneglycol divinylether (TDE), purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Initiator is peroxidized t-butyl perbenzoate (TBPB), purchased from Sigma-Aldrich (Shanghai) trade Co., Ltd.
Vegetable fibre strengthens environmentally friendly UPE matrix material:
Environmentally friendly UPE resin is obtained than blended solid without vinylbenzene UPE and reactive solvents by certain quality.Vegetable fibre, environmentally friendly UPE resin and initiator are strengthened environmentally friendly UPE matrix material by the hot-forming vegetable fibre that obtains.Reactive solvents is TDE, and the preparation process of environmentally friendly UPE resin is: solid is ground to 80 ~ 100 order powder without vinylbenzene UPE 50g for subsequent use; Reactive solvents TDE 50g is placed in after flask heats under 75 DEG C of water-baths, slowly adds solid and dissolves completely to it without magnetic agitation after vinylbenzene UPE powder; Taking-up is cooled to room temperature, namely obtains environmentally friendly UPE resin; The solid adopted is m-phthalic acid type UPE without vinylbenzene UPE, is synthesized obtain by propylene glycol, m-phthalic acid and FUMARIC ACID TECH GRADE.
Composite material and preparation method thereof: vegetable fibre is through shredding and after being cut into 20 cm × 20 cm fibrefelts, be dried to over dry at being placed in 100 ~ 105 DEG C; Take environmentally friendly UPE resin 75 g and initiator 3.75 g mix and blend 2min, obtain environmentally friendly UPE resin mixture liquor; By 5 ~ 9 vegetable fibre felts, (75 g) are arranged into fibre mat by orthogonal directions is superimposed, two surfaces of rapid for resin mixture liquor even application in fibre mat, then to move in punching block and to cold pressing 5min with the pressure of 6MPa at 70 DEG C, make resin penetration enter in fibre mat; Then thermocompressor is warming up to 160 DEG C of hot pressing 30min under 6MPa pressure; Hot pressing completes the heat insulation pressurize 60min of rear mold, makes it to naturally cool to room temperature.
In described preparation process, reactive solvents and solid, without the amount ratio of vinylbenzene UPE, are 1:1 according to mass ratio; The amount ratio 1: 1 of vegetable fibre and environmentally friendly UPE resin; The consumption of initiator is 5% of environmentally friendly UPE resin quality.
Composite panel Mechanics Performance Testing:
Composite panel makes dumbbell shape sample (specification: long 80mm, the wide 15mm in two ends, middle wide 10mm, gauge length 50mm, thickness 3mm) to test tensile property; The test sample of bending property is strip (specification: 60 mm × 11 mm × 3mm); The test sample of shock strength is strip (specification: 80 mm × 10 mm × 3mm).Tensile strength test is carried out according to ASTM D3039-08 standard; Flexural strength and modulus are tested and are carried out according to ASTM D790-10 standard; Shock strength test is according to GB/T1043-93.Tensile property and bending property test complete on microcomputer controlled electronic universal tester, and shock strength test completes on balance weight impact testing machine.
The tensile strength of matrix material
Known by Fig. 1, compared with the resin composite materials (tensile strength is 83.47MPa) being UPE solvent with 40% vinylbenzene, employing 40% and 50%TDE are that the resin composite materials of UPE solvent has suitable tensile strength, are respectively 78.65MPa and 77.18MPa.
The flexural strength of matrix material
Known by Fig. 2, being respectively 139.27MPa, 122.46MPa and 109.80MPa with the resin composite materials flexural strength that 40% vinylbenzene, 40%TDE and 50%TDE are UPE solvent, is that the resin composite materials flexural strength of solvent is low compared with the resin composite materials taking vinylbenzene as solvent with TDE.
The modulus in flexure of matrix material
Known by Fig. 2, being respectively 8738.40MPa, 7634.83MPa and 6885.66MPa with the resin composite materials modulus in flexure that 40% vinylbenzene, 40%TDE and 50%TDE are UPE solvent, is that the resin composite materials modulus in flexure of solvent is low compared with the resin composite materials taking vinylbenzene as solvent with TDE.
The shock strength of matrix material
Known by Fig. 3, be respectively 18.86kJ/m with the resin composite materials shock strength that 40% vinylbenzene, 40%TDE and 50%TDE are UPE solvent
2, 20.35kJ/m
2and 21.64kJ/m
2.Compared with the resin composite materials being solvent with vinylbenzene, employing 40% and 50%TDE are that the resin composite materials shock strength of solvent improves 7.9% and 14.7% respectively.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. an environmentally friendly unsaturated polyester resin, is characterized in that: obtained by the feed composition of following mass fraction: solid is without vinylbenzene unsaturated polyester 40 ~ 60 parts, reactive solvents 40 ~ 60 parts.
2. environmentally friendly unsaturated polyester resin according to claim 1, is characterized in that: described solid is m-phthalic acid type unsaturated polyester resin without vinylbenzene unsaturated polyester; Described reactive solvents is triethyleneglycol divinylether.
3. prepare a method for environmentally friendly unsaturated polyester resin as claimed in claim 1, it is characterized in that: solid is ground to 80 ~ 100 order powder without vinylbenzene unsaturated polyester; Reactive solvents heats in 75 DEG C of water-baths, slowly adds solid and dissolves completely to it without magnetic agitation after vinylbenzene unsaturated polyester powder; Taking-up is cooled to room temperature, obtains environmentally friendly unsaturated polyester resin.
4. vegetable fibre strengthens an environmentally friendly unsaturated polyester composite, it is characterized in that: obtained by the feed composition of following mass fraction: 80 ~ 100 parts, vegetable fibre, environmentally friendly unsaturated polyester resin 80 ~ 100 parts, initiator 3 ~ 7 parts.
5. vegetable fibre according to claim 4 strengthens environmentally friendly unsaturated polyester composite, it is characterized in that: described vegetable fibre is hemp fibre; Described environmentally friendly unsaturated polyester resin adopts reactive solvents and solid to obtain without vinylbenzene unsaturated polyester high-temperature blending; Described initiator is peroxidized t-butyl perbenzoate.
6. vegetable fibre according to claim 5 strengthens environmentally friendly unsaturated polyester composite, it is characterized in that: described solid is m-phthalic acid type unsaturated polyester resin without vinylbenzene unsaturated polyester; Described reactive solvents is triethyleneglycol divinylether.
7. prepare the method that vegetable fibre as claimed in claim 4 strengthens environmentally friendly unsaturated polyester composite for one kind, it is characterized in that: after environmentally friendly unsaturated polyester resin and initiator mix and blend, even application, in the upper and lower surface of vegetable fibre slab, obtains vegetable fibre by manual compression molding of mating formation and strengthens environmentally friendly unsaturated polyester composite.
8. method according to claim 7, is characterized in that: concrete steps are as follows:
(1) vegetable fibre after being cut into 20 cm × 20 cm fibrefelts, is dried to over dry at being placed in 100 ~ 105 DEG C through shredding;
(2) 40 ~ 60 parts of solids are ground to 80 ~ 100 order powder without vinylbenzene unsaturated polyester; 40 ~ 60 parts of reactive solvents heat in 75 DEG C of water-baths, slowly add solid and dissolve completely to it without magnetic agitation after vinylbenzene unsaturated polyester powder; Taking-up is cooled to room temperature, namely obtains environmentally friendly unsaturated polyester resin;
(3) by environmentally friendly unsaturated polyester resin and initiator mix and blend 2min, environmentally friendly unsaturated polyester resin mixed liquid is obtained; The vegetable fibre felt of 5 ~ 9 steps (1) is arranged into fibre mat by orthogonal directions is superimposed, two surfaces of rapid for resin mixture liquor even application in fibre mat, then to cold pressing 4 ~ 6min with the pressure of 5 ~ 7MPa at 70 DEG C, make resin penetration enter in fibre mat; Be warming up to 150 ~ 170 DEG C of hot pressing 20 ~ 40min under 5 ~ 7MPa pressure; Heat insulation pressurize 30 ~ 90min, and make it to naturally cool to room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111478A (en) * | 2015-09-09 | 2015-12-02 | 福建农林大学 | Epoxy-monomer-modified bamboo-fibril-reinforced unsaturated polyester composite material |
| CN105622858A (en) * | 2015-12-31 | 2016-06-01 | 华东理工大学华昌聚合物有限公司 | Environment-friendly styrene-free unsaturated polyester resin synthesis method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5360863A (en) * | 1992-08-11 | 1994-11-01 | Bayer Aktiengesellschaft | Radiation curable compositions and their use |
| CN104262921A (en) * | 2014-09-18 | 2015-01-07 | 福建农林大学 | Bamboo fiber reinforced styrene-free unsaturated polyester composite material and preparation method thereof |
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2015
- 2015-01-23 CN CN201510034264.3A patent/CN104628966B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5360863A (en) * | 1992-08-11 | 1994-11-01 | Bayer Aktiengesellschaft | Radiation curable compositions and their use |
| CN104262921A (en) * | 2014-09-18 | 2015-01-07 | 福建农林大学 | Bamboo fiber reinforced styrene-free unsaturated polyester composite material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111478A (en) * | 2015-09-09 | 2015-12-02 | 福建农林大学 | Epoxy-monomer-modified bamboo-fibril-reinforced unsaturated polyester composite material |
| CN105111478B (en) * | 2015-09-09 | 2017-11-21 | 福建农林大学 | A kind of epoxy monomer is modified bamboo fiber enhancing unsaturated polyester composite |
| CN105622858A (en) * | 2015-12-31 | 2016-06-01 | 华东理工大学华昌聚合物有限公司 | Environment-friendly styrene-free unsaturated polyester resin synthesis method |
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