CN102634039A - Pretreatment method of native cellulose fibers for reinforced composite - Google Patents
Pretreatment method of native cellulose fibers for reinforced composite Download PDFInfo
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- CN102634039A CN102634039A CN2012101200171A CN201210120017A CN102634039A CN 102634039 A CN102634039 A CN 102634039A CN 2012101200171 A CN2012101200171 A CN 2012101200171A CN 201210120017 A CN201210120017 A CN 201210120017A CN 102634039 A CN102634039 A CN 102634039A
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Abstract
The invention discloses a pretreatment method of native cellulose fibers for a reinforced composite. Through the procedures of temperature and humidity balance, high-temperature high-pressure treatment, swelling treatment, ultrasonic treatment and the like on natural fibers, the pretreatment method can be used for opening entanglements of molecular chains of defect structures and amorphous regions of the natural fibers, eliminating weak and strong parts of the natural fibers while forming tiny hairiness structures on the surfaces of the natural fibers, improving the interfacial compatibility between the natural fibers and matrices of the composite and enhancing the dispersion degree of a natural fiber composite material, thereby providing conditions for preparing the natural fiber reinforced composite with high mechanical capacity.
Description
Technical field
The invention belongs to field of materials.It relates to the pretreatment process of a kind of reinforced composite with natural fiber, and especially a kind of reinforced composite is with the pretreatment process of native cellulose fibre.
Background technology
Natural fiber is very abundant in the occurring in nature resource, and it mainly comprises bar stem fibrid (bamboo and wood, bagasse, sorghum rod, straw etc.), fruit fibrid (Exocarpium cocois (Cocos nucifera L), Pericarppium arachidis hypogaeae etc.), bast fibers (flax, jute, hemp, Zhu fiber crops etc.), leaf fibrid (sisal hemp, reed, cogongrass etc.).Natural-fiber composite material is made up of natural fiber and thermoset or resin matrix, and fiber is dispersed in the matrix as strengthening body, plays topmost carrying effect.Compare with glass fibre reinforced composion, natural-fiber composite material has that density is low, soundproof effect good,, advantage such as human body affinity good higher, recyclable, cheap than performance, thereby received the very big concern in market.
But, because the melt viscosity of resin (is generally 500～5000PaS) and generally all surpasses 100PaS, therefore in the course of processing, be unfavorable for the distribution of fortifying fibre and the dipping of matrix resin.In the process of preparation flaxen fiber reinforced composite, remain in following two problems: the consistency of (1) flaxen fiber and resin matrix is poor; (2) bad dispersibility of flaxen fiber in resin.For the mechanical property of reinforced composite, general method is to handle through physics or chemical process to strengthen material, improves the interfacial bond property that strengthens between the material base material and achieves the goal.Surface of natural fibers is handled domestic method can be divided into physics method and chemical method.The physics method mainly contains: cold gas ions method and autoclaving.Cold gas ions method can change the fiber surface oxidizing property, thereby changes surface energy.Autoclaving is a kind of wet heat treatment method, and this method can reduce the water-absorbent of fiber, thereby improves the interface behavior of material.Chemical method mainly contains: alkali lye is handled, silane treatment, and the processing of second phthalein, benzene first phthalein is handled, and the acrylonitrile grafting is handled, and permanganic acid is handled, peroxide treatment, isocyanic acid is handled, and Triple Pressed Stearic Acid is handled, and Youxiaolin is handled.Adopting interfacial compatibilizer also is another important method of improving consistency.But in treating processes, there is the mechanical property decline problem that significantly causes owing to structure deterioration in these natural fibers.And these treatment processs also fail fundamentally to improve the problem of the interface compatibility difference between natural fiber and the matrix material.
In addition, stronger hydrogen bonded causes the difficult dispersion of fiber between the natural fiber, and the fiber add-on is many more, just disperses all the more difficulty; Cellulosic molecular weight has polymolecularity, the performance heterogeneity, and be by staggered two phase systems that form that connect of crystallizing field and pars amorpha, wherein also have many pore textures.These two kinds of factors are from also caused the low problem of natural fiber and matrix consistency mechanical property poor, matrix material in essence.
Therefore, being necessary to seek a kind of dispersiveness and the natural fiber treatment process of interface compatibility of natural fiber in matrix material of can improving is very important.
Summary of the invention
The purpose of this invention is to provide the pretreatment process of a kind of reinforced composite with natural fiber, especially a kind of reinforced composite is with the pretreatment process of native cellulose fibre.The characteristics of this pretreatment process are to tangle through the molecule segment of opening natural fiber defect structure and pars amorpha; A little less than eliminating natural fiber in the powerful position; Form tiny filoplume structure in surface of natural fibers; Improve natural fiber and the interface compatibility of matrices of composite material and the degree of scatter in the natural-fiber composite material, thereby be that the natural fiber reinforced composite for preparing high-mechanical property provides condition.
The technical scheme of technical solution problem of the present invention is following:
A kind of reinforced composite is characterized in that with the pretreatment process of native cellulose fibre it comprises following step:
(1) regain with natural fiber is adjusted to 30～60%, is incubated 1～5 hour down at 100 ℃;
(2) natural fiber of step (1) being handled is 150～180 ℃ in temperature, and pressure is pressurize 2～5 minutes under the condition of 1.0～1.5MPa, and release of pressure is fast opened the rejected region of natural fiber;
(3) will pass through the natural fiber that step (2) handles and immerse fully in the natural fiber swelling agent, carry out swelling treatment, open the entanglement of natural fiber pars amorpha and fiber rejected region molecule segment;
(4) will clean through the natural fiber that step (3) is handled after, immerse in the water, be that 20～40KHz, power are supersound process 5～60 minutes under 300～2400W condition in ultrasonic frequency, the molecule segment of further opening the natural fiber pars amorpha tangles;
The natural fiber that (5) will pass through step (4) carries out drying, and is subsequent use.
Natural fiber of the present invention comprises cotton fibre, bombax cotton, ramee, flax fiber, tossa, hemp fibre, apocynum fibre, bamboo fibers, stalk fibre, sisal fibers, banana fiber, abaca fibre, coir, lotus root fibre, Folium Phragmitis fiber, Leaf of Lalang Grass fiber.
The described natural fiber swelling treatment of step (3) can adopt a kind of in the following method:
(a) being that 10～20% sodium hydroxide solution is the natural fiber swelling agent with mass percent concentration, was under-10～20 ℃ of conditions in temperature, with natural fiber dip treating 10～120 minutes.
(b) being that the aqueous solution of N-methylmorpholine-N-oxide compound (NMMO) of 20～80% is the natural fiber swelling agent with mass percentage content, was under 60～80 ℃ of conditions in temperature, with natural fiber dip treating 30～120 minutes.
(c) with the aqueous solution that contains mass percentage content 4～5% Lithium Hydroxide MonoHydrates and 10～15% thiocarbamides or urea as the natural fiber swelling agent, under temperature-5～20 ℃ condition, with natural fiber dip treating 10～60 minutes.
(d) with water ratio be 2～5% 1-butyl-tri-methylimidazolium villaumite or allyl group-3-Methylimidazole villaumite ionic liquid; Or water ratio is that 1-ethyl-3-Methylimidazole acetate ionic liquid of 10～15% is the natural fiber swelling agent; In temperature was under 80～110 ℃ of conditions, with natural fiber dip treating 3～30 minutes.
The invention has the beneficial effects as follows:
Molecule segment through opening natural fiber defect structure and pars amorpha tangles; Powerful position a little less than the elimination natural fiber; Form tiny filoplume structure in surface of natural fibers; Improve the interface compatibility of natural fiber and matrices of composite material, improve the degree of scatter of natural fiber in matrix material, thereby be that the natural fiber reinforced composite for preparing high-mechanical property provides condition.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, should be understood that these embodiment only limit to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can make various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalences fall within the application's appended claims institute restricted portion equally.
Embodiment 1
A kind of reinforced composite is characterized in that with the pretreatment process of ramee it comprises following step:
(1) regain with ramee is adjusted to 60%, is incubated 3 hours down at 100 ℃;
(2) ramee of step (1) being handled is 160 ℃ in temperature, and pressure is pressurize 3 minutes under the condition of 1.5MPa, and release of pressure is fast opened the rejected region of ramee;
(3) will pass through the ramee that step (2) handles and immerse fully in the swelling agent, carry out swelling treatment, open the entanglement of ramee pars amorpha and fiber rejected region molecule segment;
(4) will after the ramee cleaning that step (3) is handled, immersing in the water, is that 20KHz, power are under the 500W condition in ultrasonic frequency, supersound process 50 minutes, and the molecule segment of further opening the ramee pars amorpha tangles;
The ramee that (5) will pass through step (4) carries out drying, and is subsequent use.
The described ramee swelling treatment of step (3) method is:
With mass percent concentration was that 12% sodium hydroxide solution is the ramee swelling agent, is under-5 ℃ of conditions in temperature, with ramee dip treating 30 minutes.
Embodiment 2
A kind of reinforced composite is characterized in that with the pretreatment process of bamboo fibers it comprises following step:
(1) regain with bamboo fibers is adjusted to 45%, is incubated 5 hours down at 100 ℃;
(2) bamboo fibers of step (1) being handled is 180 ℃ in temperature, and pressure is pressurize 2 minutes under the condition of 1.2MPa, and release of pressure is fast opened the rejected region of bamboo fibers;
(3) will pass through the bamboo fibers that step (2) handles and immerse fully in the swelling agent, carry out swelling treatment, open the entanglement of bamboo fibers pars amorpha and fiber rejected region molecule segment;
(4) will after the bamboo fibers cleaning that step (3) is handled, immersing in the water, is that 30KHz, power are under the 1000W condition in ultrasonic frequency, supersound process 40 minutes, and the molecule segment of further opening the bamboo fibers pars amorpha tangles;
The bamboo fibers that (5) will pass through step (4) carries out drying, and is subsequent use.
The described bamboo fibers swelling treatment of step (3) method is:
The aqueous solution that with mass percentage content is N-methylmorpholine-N-oxide compound (NMMO) of 50% was the natural fiber swelling agent, is under 70 ℃ of conditions in temperature, with bamboo fibers dip treating 60 minutes.
Embodiment 3
A kind of reinforced composite is characterized in that with the pretreatment process of coir it comprises following step:
(1) regain with coir is adjusted to 35%, is incubated 4 hours down at 100 ℃;
(2) coir of step (1) being handled is 170 ℃ in temperature, and pressure is pressurize 5 minutes under the condition of 1.5MPa, and release of pressure is fast opened the rejected region of coir;
(3) will pass through the coir that step (2) handles and immerse fully in the swelling agent, carry out swelling treatment, open the entanglement of coir pars amorpha and fiber rejected region molecule segment;
(4) will after the coir cleaning that step (3) is handled, immersing in the water, is that 40KHz, power are under the 2400W condition in ultrasonic frequency, supersound process 10 minutes, and the molecule segment of further opening the coir pars amorpha tangles;
The coir that (5) will pass through step (4) carries out drying, and is subsequent use.
The described coir swelling treatment of step (3) method is:
With the aqueous solution that contains mass percentage content 4.5% Lithium Hydroxide MonoHydrate and 12% thiocarbamide as the natural fiber swelling agent, under temperature-5 ℃ condition, with coir dip treating 30 minutes.
Embodiment 4
A kind of reinforced composite is characterized in that with the pretreatment process of banana leaf fiber it comprises following step:
(1) regain with the banana leaf fiber is adjusted to 30%, is incubated 3 hours down at 100 ℃;
(2) the banana leaf fiber of step (1) being handled is 180 ℃ in temperature, and pressure is pressurize 4 minutes under the condition of 1.5MPa, and release of pressure is fast opened the rejected region of banana leaf fiber;
(3) will pass through the banana leaf fiber that step (2) handles and immerse fully in the swelling agent, carry out swelling treatment, open the entanglement of banana leaf fiber pars amorpha and fiber rejected region molecule segment;
(4) will after the banana leaf fiber cleaning that step (3) is handled, immersing in the water, is that 30KHz, power are under the 1200W condition in ultrasonic frequency, supersound process 15 minutes, and the molecule segment of further opening banana leaf fiber pars amorpha tangles;
The banana leaf fiber that (5) will pass through step (4) carries out drying, and is subsequent use.
The described banana leaf fiber of step (3) swelling treatment method is:
With water ratio is that allyl group-3-Methylimidazole villaumite ionic liquid of 3% is the natural fiber swelling agent, is under 85 ℃ of conditions in temperature, and the banana leaf fiber impregnation was handled 10 minutes.
Claims (3)
1. a reinforced composite is characterized in that with the pretreatment process of native cellulose fibre it comprises following step:
(1) regain with natural fiber is adjusted to 30～60%, is incubated 1～5 hour down at 100 ℃;
(2) natural fiber of step (1) being handled is 150～180 ℃ in temperature, and pressure is pressurize 2～5 minutes under the condition of 1.0～1.5MPa, and release of pressure is fast opened the rejected region of natural fiber;
(3) will pass through the natural fiber that step (2) handles and immerse fully in the natural fiber swelling agent, carry out swelling treatment, open the entanglement of natural fiber pars amorpha and fiber rejected region molecule segment;
(4) will clean through the natural fiber that step (3) is handled after, immerse in the water, be that 20～40KHz, power are supersound process 5～60 minutes under 300～2400W condition in ultrasonic frequency, the molecule segment of further opening the natural fiber pars amorpha tangles;
The natural fiber that (5) will pass through step (4) carries out drying, and is subsequent use.
2. a kind of reinforced composite according to claim 1 is characterized in that with the pretreatment process of native cellulose fibre described natural fiber comprises cotton fibre, bombax cotton, ramee, flax fiber, tossa, hemp fibre, apocynum fibre, bamboo fibers, stalk fibre, sisal fibers, any of several broadleaf plants leaf fibres, coir, lotus root fibre, Folium Phragmitis fiber, Leaf of Lalang Grass fiber.
3. a kind of reinforced composite according to claim 1 is with the pretreatment process of native cellulose fibre, it is characterized in that the described natural fiber swelling treatment of step (3) can adopt a kind of in the following method:
(a) being that 10～20% sodium hydroxide solution is the natural fiber swelling agent with mass percent concentration, was under-10～20 ℃ of conditions in temperature, with natural fiber dip treating 10～120 minutes.
(b) being that the aqueous solution of N-methylmorpholine-N-oxide compound (NMMO) of 20～80% is the natural fiber swelling agent with mass percentage content, was under 60～80 ℃ of conditions in temperature, with natural fiber dip treating 30～120 minutes.
(c) with the aqueous solution that contains mass percentage content 4～5% Lithium Hydroxide MonoHydrates and 10～15% thiocarbamides or urea as the natural fiber swelling agent, under temperature-5～20 ℃ condition, with natural fiber dip treating 10～60 minutes.
(d) with water ratio be 2～5% 1-butyl-tri-methylimidazolium villaumite or allyl group-3-Methylimidazole villaumite ionic liquid; Or water ratio is that 1-ethyl-3-Methylimidazole acetate ionic liquid of 10～15% is the natural fiber swelling agent; In temperature was under 80～110 ℃ of conditions, with natural fiber dip treating 3～30 minutes.
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Cited By (9)
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| CN103709773A (en) * | 2013-12-12 | 2014-04-09 | 湖北工业大学 | Alkaline thiourea disentangled straw/resin composite board making method |
| CN105175342A (en) * | 2015-10-14 | 2015-12-23 | 大连工业大学 | Ionic liquid and method for homogeneous phase-modified reed-reinforced PE (polyethylene) composite material thereof |
| CN105484025A (en) * | 2015-12-24 | 2016-04-13 | 西南大学 | Prickle and itch feeling-resisting finishing method for ramie fabric by imidazole ionic liquid |
| CN105506779A (en) * | 2016-01-13 | 2016-04-20 | 江苏科技大学 | Mulberry and bamboo composite fibers obtained after graft modification of mulberry fibers and bamboo fibers in ionic liquid and preparation method thereof |
| CN107903649A (en) * | 2017-12-01 | 2018-04-13 | 李晨阳 | A kind of degradable sorghum husk micro mist/polylactic acid composite modification material and preparation method thereof |
| CN111040449A (en) * | 2019-12-26 | 2020-04-21 | 合肥中汇睿能能源科技有限公司 | Modified polyimide film and preparation method thereof |
| CN112171830A (en) * | 2020-09-15 | 2021-01-05 | 南京大学 | High-strength wood and preparation method thereof |
| CN112178096A (en) * | 2020-09-15 | 2021-01-05 | 南京大学 | Wood spring and preparation method thereof |
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2012
- 2012-04-18 CN CN2012101200171A patent/CN102634039A/en active Pending
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| CN103709773B (en) * | 2013-12-12 | 2016-02-10 | 湖北工业大学 | The preparation method of alkali urea disentanglement stalk/resin composite plates |
| CN103709773A (en) * | 2013-12-12 | 2014-04-09 | 湖北工业大学 | Alkaline thiourea disentangled straw/resin composite board making method |
| CN105175342B (en) * | 2015-10-14 | 2018-07-20 | 大连工业大学 | A kind of method of ionic liquid and its homogeneous modified reed enhancing PE composite materials |
| CN105175342A (en) * | 2015-10-14 | 2015-12-23 | 大连工业大学 | Ionic liquid and method for homogeneous phase-modified reed-reinforced PE (polyethylene) composite material thereof |
| CN105484025A (en) * | 2015-12-24 | 2016-04-13 | 西南大学 | Prickle and itch feeling-resisting finishing method for ramie fabric by imidazole ionic liquid |
| CN105506779A (en) * | 2016-01-13 | 2016-04-20 | 江苏科技大学 | Mulberry and bamboo composite fibers obtained after graft modification of mulberry fibers and bamboo fibers in ionic liquid and preparation method thereof |
| CN107903649A (en) * | 2017-12-01 | 2018-04-13 | 李晨阳 | A kind of degradable sorghum husk micro mist/polylactic acid composite modification material and preparation method thereof |
| CN111040449A (en) * | 2019-12-26 | 2020-04-21 | 合肥中汇睿能能源科技有限公司 | Modified polyimide film and preparation method thereof |
| CN112171830A (en) * | 2020-09-15 | 2021-01-05 | 南京大学 | High-strength wood and preparation method thereof |
| CN112178096A (en) * | 2020-09-15 | 2021-01-05 | 南京大学 | Wood spring and preparation method thereof |
| CN112171830B (en) * | 2020-09-15 | 2022-06-21 | 南京大学 | High-strength wood and preparation method thereof |
| CN116082778A (en) * | 2023-03-02 | 2023-05-09 | 江苏盈美复合材料有限公司 | Flame-retardant natural fiber reinforced thermoplastic composite material and manufacturing method thereof |
| CN116082778B (en) * | 2023-03-02 | 2024-04-26 | 江苏盈韧新材料科技有限公司 | Flame-retardant natural fiber reinforced thermoplastic composite material and manufacturing method thereof |
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Application publication date: 20120815 |