CN103709773A - Alkaline thiourea disentangled straw/resin composite board making method - Google Patents
Alkaline thiourea disentangled straw/resin composite board making method Download PDFInfo
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- CN103709773A CN103709773A CN201310672086.8A CN201310672086A CN103709773A CN 103709773 A CN103709773 A CN 103709773A CN 201310672086 A CN201310672086 A CN 201310672086A CN 103709773 A CN103709773 A CN 103709773A
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Abstract
The invention discloses an alkaline thiourea disentangled straw/resin composite board making method. The method comprises the following steps: sprinkling short fibers of straws with a pre-cooled aqueous NaOH solution, and stirring and kneading for 30min-2h; sprinkling the short fibers with a pre-cooled aqueous urea solution, and continuously stirring and kneading for 30min-2h; drying, and crushing to 60 mesh powder to obtain alkaline thiourea disentangled straw fibers; and blending the obtained alkaline thiourea disentangled straw with resin, a compatilizer, a lubricant and a filler, compacting or extruding, and carrying out continuous production to obtain alkaline thiourea disentangled straw/resin composite boards. The alkaline thiourea disentangled straw/resin composite boards made by utilizing the method can be widely applied to the fields of building materials, decoration materials, packaging materials and the like because of the advantages of light weight, low price, good strength and the like.
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 the composite sheet that 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 is to abandon and burn, and has wasted resource and has polluted again environment.In recent years, increasing scholar is devoted to research using crop plants fiber as filler or strongthener and thermoplastic polymer carry out compound research.Stalk fibre has been compared many advantages 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 has hindered the combination of polymkeric substance and stalk fibre, has formed obvious two interfacial layers that are separated.What Main Mechanical was provided in stalk fibre is Mierocrystalline cellulose, and hemicellulose, xylogen and ash content tangle, Mierocrystalline cellulose has hindered the compound of Mierocrystalline cellulose and resin matrix.And Mierocrystalline cellulose contains many oh groups, belongs to polar group, with the complete compatible surface property that needs to improve stalk fibre of nonpolar plastic substrate.In order to improve the interface performance of stalk fibre and thermoplastic resin, must carry out modification or introduce suitable interfacial compatibilizer stalk fibre or plastic substrate, make dissimilar materials easy dispersion and fusion in recombination process, form stable, firm, uniform interfacial layer.
CN102704296A discloses a kind of method of alkali lye Treating straw raw material, stalk is soaked in alkali lye to 1-3 hour, pass into again the steam 1-2 hour of 130 ℃-200 ℃, thereby reach, remove the object that lignin separation goes out Mierocrystalline cellulose and hemicellulose, this treatment process need to be used a large amount of alkali lye to soak stalk completely, and this high-temperature steam processing 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 in advance again 0-8 ℃, be stirred into soda cellulose solution, the 2wt%-40wt% aqueous solution of urea that adds again 0-15 ℃, at room temperature stir and make transparent cellulose solution, this treatment process needs a large amount of alkali lye and urea to soak Mierocrystalline cellulose, as needed to process a large amount of waste liquids for the preparation of composite sheet and easily polluting.
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 has significantly been improved stalk fibre and the compound interface compatibility of thermoplastics, has improved the mechanical property of composite sheet.
In order to realize object of the present invention, contriver studies and persistent exploration by lot of experiments, has finally obtained 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 respectively the NaOH aqueous solution of 7wt%-28wt% and the aqueous solution of urea of 14wt%-42wt%, be placed at 0 ℃ 2-5 hour until solution constant temperature to 0 ℃.
(3) the stalk quality 1-2 good NaOH aqueous solution of precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then the 1-2 of the stalk quality good aqueous solution of urea of precooling is doubly sprayed onto on staple fibre, continues to stir 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 and resin, compatilizer, lubricant and filler blend in step (3), suppresses or extrudes, and produces continuously, obtains 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 suppressed or extrude by following weight part proportioning blend:
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 single screw rod or twin screw extruder to carry out extrusion moulding.
Described stalk is the rice straw of this season harvesting, the rice straw that preferred water content is 6%-10%.
The alkali urea disentanglement stalk/resin composite plates that utilizes 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, being to untie hemicellulose, xylogen and the ash content becoming entangled on cellulose molecular chain on the one hand, is to reduce the polarity of stalk fibre and improve its physical behavior to make it can disperse preferably in plastic substrate on the other hand.Compared to the method for having reported, the present invention, without stalk is soaked completely, saves time and cost, simple to operation.The present invention wants dissolving cellulos, but at low temperatures, alkaline solution is more easily opened the hydrogen bond of Mierocrystalline cellulose and hemicellulose molecule interchain, and urea soln is that cellulose molecular chain is unfolded.Alkali urea precooling treatment stalk is to untie 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 processing of stalk fibre, by Mechanical Crushing effect, change its physical form, the surface-area that has increased stalk fibre has increased inner breakage; Then use aqueous sodium hydroxide solution and aqueous solution of urea after freezing that fiber is stirred and rubbed; this processes and compares with traditional chemical immersion; reduced the consumption of chemical reagent; saved the time; reduced the pollution of waste liquid to environment; can effectively improve the consistency of stalk fibre and plastic substrate again simultaneously; thereby 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
Fig. 1 is that stalk inner cellulose is processed the schematic diagram of disentanglement process by alkali urea.
Embodiment
The preparation method of the alkali urea disentanglement stalk/resin composite plates 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 stalk quality 1-2 good 7wt%-28wt%NaOH aqueous solution of precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then the 1-2 of the stalk quality good 14wt%-42wt% aqueous solution of urea of precooling is doubly sprayed onto on staple fibre, continues to stir 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
Alkali urea disentanglement stalk fibre and plastics is mixing on two rollers, add compatilizer, lubricant, filler etc., mix rear compacting or extrusion moulding, obtain alkali urea disentanglement stalk/resin composite plates.
Below by the comparative example of common stalk/resin composite plates and an embodiment for three alkali urea disentanglement stalk/resin composite plates who does not do any processing, technical solution of the present invention is described further, but protection scope of the present invention is not limited to these examples.Every do not deviate from the change of inventive concept or be equal to substitute 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 and be broken into 60 object powder and add in 50 parts of HDPE, add 1 part of maleic anhydride grafted polyethylene, 2 parts of Zinic stearass, 1.3 parts of compression mouldings after two rods are begun to pratise of titanium dioxide, obtain stalk/resin composite plates.The composite materials property obtaining 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.80 parts of good 14wt%NaOH aqueous solution of precooling are sprayed onto on 50 parts of stalk staple fibres, stir and rub 30 minutes; Then the good 28wt% aqueous solution of urea of the precooling of 80 parts is sprayed onto on staple fibre, continues to stir 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, add 1 part of maleic anhydride grafted polyethylene, 2 parts of Zinic stearass, 1.3 parts of compression mouldings after two rods are begun to pratise of titanium dioxide, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtaining 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 good 14wt%NaOH aqueous solution of the precooling of 50 parts is sprayed onto on 30 parts of stalk staple fibres, stirs and rub 30 minutes; Then the good 28wt% aqueous solution of urea of the precooling of 50 parts is sprayed onto on staple fibre, continues to stir 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, add 1 part of maleic anhydride grafted polyethylene, 2 parts of Zinic stearass, 1.3 parts of compression mouldings after two rods are begun to pratise of titanium dioxide, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtaining 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 good 14wt%NaOH aqueous solution of the precooling of 80 parts is sprayed onto on 40 parts of stalk staple fibres, stirs and rub 30 minutes; Then the good 28wt% aqueous solution of urea of the precooling of 80 parts is sprayed onto on staple fibre, continues to stir 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, add 1 part of maleic anhydride grafted polyethylene, 1 part of Zinic stearas, 1.3 parts of compression mouldings after two rods are begun to pratise of titanium dioxide, obtain alkali urea disentanglement stalk/resin composite plates.The composite materials property obtaining is as table 1.
The mechanical performance compare of stalk/resin composite plates prepared by table 1 comparative example and each embodiment
Alkali urea disentanglement stalk/resin composite plates of preparing according to embodiment, its physical properties all has significantly lifting after testing, tensile strength is brought up to 19.2MPa by original 11.5MPa, and flexural strength rises to 25.1 by original 20.7, and shock strength is by 4.2 original KJ/m
2rise to 6.0 KJ/m
2.And the performance that alkali urea disentanglement stalk/resin composite plates also has is ageing-resistant, water absorbability is little and can repeat to recycle, 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 (9)
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, standby;
(2) aqueous solution of urea that the NaOH aqueous solution that compound concentration is 7wt%-28wt% respectively and concentration are 14wt%-42wt%, is placed at 0 ℃ 2-5 hour until solution constant temperature to 0 ℃ is standby;
(3) the stalk quality 1-2 good NaOH aqueous solution of precooling is doubly sprayed onto on staple fibre, stirs and rub 30 minutes to 2 hours; Then the 1-2 of the stalk quality good aqueous solution of urea of precooling is doubly sprayed onto on staple fibre, continues to stir and rub 30 minutes to 2 hours; Finally staple fibre is dried and is crushed to 60 object powder, obtain alkali urea disentanglement stalk fibre, standby;
(4) by alkali urea disentanglement stalk fibre and resin, compatilizer, lubricant and filler blend, suppress or extrude, produce continuously, obtain alkali urea disentanglement stalk/resin composite plates.
2. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1, it is characterized in that: described alkali urea disentanglement stalk fibre and resin, compatilizer, lubricant and filler are suppressed or extrude by following weight part proportioning blend:
Alkali urea disentanglement stalk fibre 30-70 part
Resin 30-70 part
Compatilizer 1-2 part
Lubricant 1-5 part
Filler 1-5 part.
3. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it is characterized in that: described resin is: the co-mixing system of polyethylene, polypropylene, polyvinyl chloride or several thermoplasticss or waste or used plastics.
4. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it 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.
5. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it is characterized in that: described lubricant is selected from following one or more: stearic acid, Zinic stearas, calcium stearate, PE wax, paraffin.
6. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it is characterized in that: described filler is selected from following one or more: talcum powder, calcium carbonate, silicon-dioxide, titanium dioxide, polynite, mica.
7. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it is characterized in that: described being compressed to used hot pressing and colded pressing and be pressed; Described extrudes as using single screw rod or twin screw extruder to carry out extrusion moulding.
8. according to the preparation method of the alkali urea disentanglement stalk/resin composite plates of claim 1 or 2, it is characterized in that: described stalk is the rice straw of this season harvesting.
9. the preparation method of alkali urea disentanglement stalk/resin composite plates according to Claim 8, is characterized in that: described stalk water content is 6%-10%.
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| CN107987478A (en) * | 2017-12-13 | 2018-05-04 | 衢州瀚心科技有限公司 | Rice hull cellulose synthetic resin material and preparation method thereof |
| CN109735070A (en) * | 2018-12-12 | 2019-05-10 | 宁波大学 | A kind of polylactic acid/bamboo particle/bamboo charcoal composite material preparation method |
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| 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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