CN103709773B - The preparation method of alkali urea disentanglement stalk/resin composite plates - Google Patents
The preparation method of alkali urea disentanglement stalk/resin composite plates Download PDFInfo
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- CN103709773B CN103709773B CN201310672086.8A CN201310672086A CN103709773B CN 103709773 B CN103709773 B CN 103709773B CN 201310672086 A CN201310672086 A CN 201310672086A CN 103709773 B CN103709773 B CN 103709773B
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Abstract
The invention discloses a kind of preparation method of alkali urea disentanglement stalk/resin composite plates, the method is sprayed onto on stalk staple fibre by the NaOH aqueous solution good for precooling, stirs and rub 30 minutes to 2 hours; Then the aqueous solution of urea that precooling is good is sprayed onto on staple fibre, continues stirring and rub 30 minutes to 2 hours; Be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre after dry; The alkali urea disentanglement stalk fibre of gained and resin, compatilizer, lubricant, filler is blended, suppress or extrude, carry out continuous seepage, obtain alkali urea disentanglement stalk/resin composite plates.The alkali urea disentanglement stalk/resin composite plates utilizing the inventive method to prepare, so that its light weight, cheapness and intensity is better etc., advantage can be widely used in the fields such as material of construction, finishing material, wrapping material.
Description
Technical field
The present invention relates to a kind of stalk fibrous composite, particularly the composition board preparation method of a kind of alkali urea disentanglement stalk fibre and resin, belongs to Material cladding technical field.
Background technology
Alkali urea disentanglement stalk/resin composite plates is composite sheet stalk fibre and thermoplastics are composited, and is the novel material that product quality was recycled, improved to a kind of agricultural wastes.China, as large agricultural country, has abundant agronomic crop fibre resource, and wherein the average annual output of wheat straw and straw reaches 2.4 hundred million tons more than.The traditional treatment method of these agricultural wastes abandons and burns, and wastes resource and pollute environment again.In recent years, increasing scholar is devoted to study research crop plants fiber being carried out compound as filler or strongthener and thermoplastic polymer.Stalk fibre has many advantages compared with synthon, as cheap, be easy to get, density is low, power consumption of polymer processing is little and to environment and human body without harm, therefore adopt stalk fibre to replace synthon to prepare matrix material and there is significant economic implications and social effect.。
The main composition component of stalk fibre is Mierocrystalline cellulose, hemicellulose, xylogen and ash content, its surface coverage one deck wax layer.Wax layer hinders the combination of polymkeric substance and stalk fibre, defines the interfacial layer of obvious two-phase laminated flow.What provide Main Mechanical in stalk fibre is Mierocrystalline cellulose, and hemicellulose, xylogen and ash content tangle, Mierocrystalline cellulose hinders the compound of Mierocrystalline cellulose and resin matrix.And Mierocrystalline cellulose contains many oh groups, belongs to polar group, completely compatible with nonpolar plastic substrate, need the surface property improving stalk fibre.In order to improve the interface performance of stalk fibre and thermoplastic resin, must modification be carried out to stalk fibre or plastic substrate or introduce suitable interfacial compatibilizer, make dissimilar materials easy dispersion and fusion in recombination process, form stable, firm, uniform interfacial layer.
CN102704296A discloses a kind of method of base extraction stalk, stalk is soaked 1-3 hour in alkali lye, pass into the steam 1-2 hour of 130 DEG C-200 DEG C again, thus reach the object that removing lignin separation goes out Mierocrystalline cellulose and hemicellulose, this treatment process needs to use a large amount of alkali lye to soak stalk completely, and this high temperature steam treatment energy consumption is too high.CN101074285A discloses a kind of method of dissolving cellulos, Mierocrystalline cellulose is dispersed in the 6wt%-14wt%LiOH aqueous solution, be chilled to 0-8 DEG C in advance again, be stirred into soda cellulose solution, add the 2wt%-40wt% aqueous solution of urea of 0-15 DEG C again, at room temperature stir obtained transparent cellulose solution, and this treatment process needs a large amount of alkali lye and urea to soak Mierocrystalline cellulose, as then needed process a large amount of waste liquid and easily pollute for the preparation of composite sheet.
Summary of the invention
In view of the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of alkali urea disentanglement stalk/resin composite plates.The method significantly improves the interface compatibility of stalk fibre and thermoplastics compound, improves the mechanical property of composite sheet.
In order to realize object of the present invention, contriver is studied and persistent exploration by lot of experiments, finally obtains following technical scheme:
A preparation method for alkali urea disentanglement stalk/resin composite plates, comprises the following steps:
(1) stalk fibre is broken into the staple fibre of 40-50mm.
(2) configure the NaOH aqueous solution of 7wt%-28wt% and the aqueous solution of urea of 14wt%-42wt% respectively, at being placed in 0 DEG C 2-5 hour until solution constant temperature is to 0 DEG C.
(3) the NaOH aqueous solution good for stalk quality 1-2 precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then aqueous solution of urea good for the 1-2 of stalk quality precooling is doubly sprayed onto on staple fibre, continues stirring and rub 30 minutes to 2 hours; Finally dry and be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre.
(4) gained alkali urea disentanglement stalk fibre is blended with resin, compatilizer, lubricant and filler in step (3), suppresses or extrudes, carry out continuous seepage, acquisition alkali urea disentanglement stalk/resin composite plates.
Object of the present invention can also realize like this: described alkali urea disentanglement stalk fibre and resin, compatilizer, lubricant and filler are by the blended compacting of following weight or extrude:
Alkali urea disentanglement stalk fibre 30-70 part
Resin 30-70 part
Compatilizer 1-2 part
Lubricant 1-5 part
Filler 1-5 part.
Described resin is: polyethylene, polypropylene, polyvinyl chloride or several thermoplastic resin system, or waste or used plastics.
Described compatilizer is selected from following one or more: Research of Grafting Malaic Anhydride Onto Polyethylene, polypropylene grafted maleic anhydride, ethylene-octene copolymer grafted maleic anhydride, acrylonitrile-butadiene-styrene copolymer grafted maleic anhydride, styrene-butadiene-styrene grafted maleic anhydride, styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride.
Described lubricant is selected from following one or more: stearic acid, Zinic stearas, calcium stearate, PE wax, paraffin.
Described filler is selected from following one or more: talcum powder, calcium carbonate, silicon-dioxide, titanium dioxide, polynite, mica.
Described being compressed to use hot pressing and colding pressing is pressed; Described extrudes as using singe screw or twin screw extruder to carry out extrusion moulding.
Described stalk is the rice straw of this season harvesting, and preferred water content is the rice straw of 6%-10%.
The alkali urea disentanglement stalk/resin composite plates utilizing method of the present invention to prepare, so that its light weight, cheapness and intensity is better etc., advantage can be widely used in the fields such as material of construction, finishing material, wrapping material.
Stalk fibre joins in thermoplastics as strongthener, make two-phase compatible and improve physicals, on the one hand to untie the hemicellulose become entangled on cellulose molecular chain, xylogen and ash content, be on the other hand reduce stalk fibre polarity and improve its physical behavior and make it can disperse preferably in plastic substrate.Compared to the method reported, the present invention, without the need to being soaked completely by stalk, saves time and cost, simple to operation.The present invention wants dissolving cellulos, but at low temperatures, alkaline solution more easily opens the hydrogen bond of Mierocrystalline cellulose and hemicellulose molecule interchain, and urea soln is then that cellulose molecular chain is unfolded.Alkali urea precooling treatment stalk unties entanglement between Mierocrystalline cellulose and hemicellulose, xylogen, ash content and abundant swollen cellulose.
Compared with prior art, the preparation method's tool that the present invention relates to alkali urea disentanglement stalk/resin composite plates has the following advantages and marked improvement: the method is in the process of stalk fibre, change its physical form by Mechanical Crushing effect, the surface-area increasing stalk fibre increases inner breakage; Then use freezing after aqueous sodium hydroxide solution and aqueous solution of urea stirring carried out to fiber rub; this is compared with traditional chemical immersion process; decrease the consumption of chemical reagent; save the time; reduce the pollution of waste liquid to environment; effectively can improve again the consistency of stalk fibre and plastic substrate simultaneously; thus improve the physical and mechanical property of matrix material; be embodied in that shock strength significantly improves, ageing-resistant, corrosion-resistant, water absorbability is minimum; and can reuse and recycling, be conducive to environment protection.
Accompanying drawing explanation
Figure is that stalk inner cellulose is by the schematic diagram of alkali urea process disentanglement process.
Embodiment
The preparation method of the alkali urea disentanglement stalk/resin composite plates that the present invention relates to mainly comprises following two large steps:
A) preparation of alkali urea disentanglement stalk fibre
Stalk fibre is broken into the staple fibre of 40-50mm; The 7wt%-28wt%NaOH aqueous solution good for stalk quality 1-2 precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then 14wt%-42wt% aqueous solution of urea good for the 1-2 of stalk quality precooling is doubly sprayed onto on staple fibre, continues stirring and rub 30 minutes to 2 hours; Finally dry and be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre.
B) alkali urea disentanglement stalk fibre and resin compounded
By alkali urea disentanglement stalk fibre and plastics mixing on two roller, add compatilizer, lubricant, filler etc., mix rear compacting or extrusion moulding, obtain alkali urea disentanglement stalk/resin composite plates.
The embodiment of the comparative example and three alkali urea disentanglement stalk/resin composite plates that do not do the common stalk/resin composite plates of any process below by one is described further technical solution of the present invention, but protection scope of the present invention is not limited to these examples.Every do not deviate from inventive concept change or equivalent substituting include within protection scope of the present invention.
The preparation of the common stalk/resin composite plates of comparative example
Get 50 parts of stalk fibres be broken into 60 object powder and add in 50 parts of HDPE, add maleic anhydride grafted polyethylene 1 part, Zinic stearas 2 parts, titanium dioxide 1.3 parts compression moulding after two rod is begun to pratise, obtain stalk/resin composite plates.The composite materials property obtained is as table 1.
The preparation of embodiment 1 alkali urea disentanglement stalk/resin composite plates
Get 50 parts of stalk fibres and be broken into 50mm staple fibre.The 14wt%NaOH aqueous solution good for 80 parts of precoolings is sprayed onto on 50 parts of stalk staple fibres, stirs and rub 30 minutes; Then 28wt% aqueous solution of urea good for the precooling of 80 parts is sprayed onto on staple fibre, continues stirring and rub 30 minutes; Finally dry and be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre.50 parts of alkali urea disentanglement stalk fibres are added in 50 parts of HDPE, adds maleic anhydride grafted polyethylene 1 part, Zinic stearas 2 parts, titanium dioxide 1.3 parts compression moulding after two rod is begun to pratise, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtained is as table 1.
The preparation of embodiment 2 alkali urea disentanglement stalk/resin composite plates
Get 30 parts of stalk fibres and be broken into 50mm staple fibre.The 14wt%NaOH aqueous solution good for the precooling of 50 parts is sprayed onto on 30 parts of stalk staple fibres, stirs and rub 30 minutes; Then 28wt% aqueous solution of urea good for the precooling of 50 parts is sprayed onto on staple fibre, continues stirring and rub 30 minutes; Finally dry and be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre.30 parts of alkali urea disentanglement stalk fibres are added in 70 parts of HDPE, adds maleic anhydride grafted polyethylene 1 part, Zinic stearas 2 parts, titanium dioxide 1.3 parts compression moulding after two rod is begun to pratise, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtained is as table 1.
The preparation of embodiment 3 alkali urea disentanglement stalk/resin composite plates
Get 40 parts of stalk fibres and be broken into 50mm staple fibre.The 14wt%NaOH aqueous solution good for the precooling of 80 parts is sprayed onto on 40 parts of stalk staple fibres, stirs and rub 30 minutes; Then 28wt% aqueous solution of urea good for the precooling of 80 parts is sprayed onto on staple fibre, continues stirring and rub 30 minutes; Finally dry and be crushed to 60 object powder and obtain alkali urea disentanglement stalk fibre.40 parts of alkali urea disentanglement stalk fibres are added in 60 parts of HDPE, adds maleic anhydride grafted polyethylene 1 part, Zinic stearas 1 part, titanium dioxide 1.3 parts compression moulding after two rod is begun to pratise, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtained is as table 1.
The mechanical performance compare of stalk/resin composite plates prepared by table 1 comparative example and each embodiment
According to alkali urea disentanglement stalk/resin composite plates prepared by embodiment, its physical properties all has and significantly promotes after testing, tensile strength brings up to 19.2MPa by original 11.5MPa, and flexural strength rises to 25.1 by original 20.7, and shock strength is by original 4.2KJ/m
2rise to 6.0KJ/m
2.And alkali urea disentanglement stalk/resin composite plates also have ageing-resistant, water absorbability is little and can repeat the performance recycled, this makes the environmental protection be applicable to the fields such as building decoration, garden landscape facilities, traffic track, automotive upholstery, wrapping material and pallet more of this composition board.
Claims (8)
1. the preparation method of alkali urea disentanglement stalk/resin composite plates, comprises the steps:
(1) stalk fibre is broken into the staple fibre of 40-50mm, for subsequent use;
(2) compound concentration is the NaOH aqueous solution of 7wt%-28wt% and concentration is respectively the aqueous solution of urea of 14wt%-42wt%, at being placed in 0 DEG C 2-5 hour until solution constant temperature is to 0 DEG C, for subsequent use;
(3) the NaOH aqueous solution good for stalk quality 1-2 precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then aqueous solution of urea good for the 1-2 of stalk quality precooling is doubly sprayed onto on staple fibre, continues stirring and rub 30 minutes to 2 hours; Finally staple fibre dried and be crushed to 60 object powder, obtaining alkali urea disentanglement stalk fibre, for subsequent use;
(4) by alkali urea disentanglement stalk fibre and resin, compatilizer, lubricant and filler blended, suppress or extrude, carry out continuous seepage, obtain alkali urea disentanglement stalk/resin composite plates;
Described alkali urea disentanglement stalk fibre and resin, compatilizer, lubricant and filler are by the blended compacting of following weight or extrude:
Alkali urea disentanglement stalk fibre 30-70 part
Resin 30-70 part
Compatilizer 1-2 part
Lubricant 1-5 part
Filler 1-5 part.
2. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described resin is: the co-mixing system of polyethylene, polypropylene, polyvinyl chloride or several thermoplastics or waste or used plastics.
3. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described compatilizer is selected from following one or more: Research of Grafting Malaic Anhydride Onto Polyethylene, polypropylene grafted maleic anhydride, ethylene-octene copolymer grafted maleic anhydride, acrylonitrile-butadiene-styrene copolymer grafted maleic anhydride, styrene-butadiene-styrene grafted maleic anhydride, styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride.
4. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described lubricant is selected from following one or more: stearic acid, Zinic stearas, calcium stearate, PE wax, paraffin.
5. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described filler is selected from following one or more: talcum powder, calcium carbonate, silicon-dioxide, titanium dioxide, polynite, mica.
6. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described being compressed to uses hot pressing and cold pressing and be pressed; Described extrudes as using singe screw or twin screw extruder to carry out extrusion moulding.
7. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 1, is characterized in that: described stalk is the rice straw of this season harvesting.
8. the preparation method of alkali urea disentanglement stalk/resin composite plates according to claim 7, is characterized in that: described stalk water content is 6%-10%.
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| CN105082309A (en) * | 2015-07-15 | 2015-11-25 | 百仪家具有限公司 | High-cost-performance and high-density fiberboard where paint can be directly sprayed and preparation method of high-cost-performance and high-density fiberboard |
| CN107760048A (en) * | 2017-10-24 | 2018-03-06 | 芜湖蓝天工程塑胶有限公司 | Stalk fibrous composite 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 |
| CN107987478B (en) * | 2017-12-13 | 2021-07-09 | 黄雪妮 | Rice hull fiber synthetic resin material and preparation method thereof |
| CN109735070B (en) * | 2018-12-12 | 2021-07-27 | 宁波大学 | Preparation method of polylactic acid/bamboo particle/bamboo charcoal composite material |
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