CN105038284A - Method for preparing wood-plastic composite material by using wood fibers - Google Patents
Method for preparing wood-plastic composite material by using wood fibers Download PDFInfo
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Abstract
The invention provides a method for preparing a wood-plastic composite material by using wood fibers. Particularly, the method comprises the following steps: 1) regulating the carbon-nitrogen ratio of dry matter wood fibers, regulating the moisture content of the dry matter wood fibers to 60-70%, adding a biological treating agent, fermenting for 5-15 days, drying in air till the moisture content reaches 12-14%; 2) adding a coupling agent and an antioxidant and mixing uniformly; 3) adding plastic and mixing uniformly; and 4) performing extrusion pelletization. According to the method, sisal dregs, bagasse, rice hull, straws, bamboo leftover and other natural wood fibers are fermented at proper carbon-nitrogen ratio and moisture content by virtue of addition of the biological treating agent; under the action of microbes, macromolecules of the wood fibers are decomposed, intermolecular forces of fibers can be reduced, and the melt index, liquidity, hydrophobicity and tensile strength of the material can be improved. The wood-plastic composite material obtained by the method can be processed into wood-plastic composite material products of various properties and shapes; moreover, the whole production process is low in energy consumption and friendly to the environment.
Description
Technical field
The invention belongs to polymeric material field, particularly a kind of method applied wood fibre and prepare wood plastic composite.
Background technology
Wood plastic composite is a kind of advanced composite material, that agriculture and forestry organic waste material (as vegetable fibres such as powdered rice hulls, straw powder, bamboo powder, wood powders) is main raw material filling, strengthens, with vinyon or recycle polyethylene plastics, through hot pressing compound, the modified thermoplastic material that different processing mode makes such as to melt extrude, be mainly used in the raw materials for production of Side fascia, fence, step, Shu Chi, flower case, rubbish container etc.Wood plastic composite has merged the two-fold advantage of vegetable fibre and plastics, the limitation that can overcome that xylon intensity is low, the large and plastic material Young's modulus of variability is low etc. causes, the vegetable fibre after discarding and plastics can be made full use of again, energy-saving and emission-reduction, reduce environmental pollution, promoting the value added of material, is a kind of type material having development prospect.
But the vegetable fibre in wood plastic composite of the prior art owing to being caused extrudate density excessive by compression in the course of processing, difficulty is brought to carrying, complete processing, contain great amount of hydroxy group in vegetable fibre structure simultaneously, these hydroxyls define molecule hydrogen bond and intermolecular hydrogen bonding, thus make vegetable fibre have stronger polarity and wetting ability, and thermoplastics majority is nonpolar, there is hydrophobicity.When both being mixed, complex systems median surface degrees of fusion is low, lacks due cohesive strength, cannot embody the mechanical property aspect advantage that it is intrinsic.
In order to address the aforementioned drawbacks, physics is adopted in production, chemistry, biological method is with the interface compatibility improved between thermoplastics and vegetable fibre and the processing fluidity improving wooden molded material: the Chinese patent being CN103193988A as publication number discloses a kind of method utilizing natural fiber material to prepare wood plastic composite, it utilizes timber, bamboo wood, the natural fiber materials such as stalk, by pulverizing, low temperature alkali lye profit rises, Benzylation, the method that feedstock conversion is thermoplastic material is fallen, make timber, bamboo wood, stalk has some characteristics of plastics and heat melts processing characteristics, wood plastic composite is made again by granulating equipment, publication number is a kind of method that the Chinese patent of CN104479223A proposes wood plastic composite utilizing staple fibre to prepare, this invention with staple fibre waste and macrofiber be strongthener, thermoplastics polymer prepares wood plastic composite for matrix, raw material is after pre-treatment, add macrofiber high-speed mixing, mechanical activation coupling solid-state modification, add plastics high-speed mixing again, plasticate, obtain wood plastic composite finally by hot-forming, publication number is the preparation method that the Chinese patent of CN104356663A discloses a kind of xylogen thermoplastic materials, biomass material is carried out the quick-fried enzymolysis again of clean vapour, obtain slag charge, by slag charge drying with after pulverizing, obtain lignin particles raw material, after last and PE mixed with resin, injection moulding extrudes, and obtains xylogen thermoplastic materials, publication number is that the Chinese patent of CN104371236A discloses a kind of organosilane crosslinked polyethylene wood plastic composite, by after drying vegetable fibers grinding and polyethylene and mix lubricant, then add the mixing of silane coupling agent, initiator, catalyzer and oxidation inhibitor, and utilize twin screw extruder to obtain organosilane crosslinked polyethylene wood plastic composite, from foregoing invention patent, still relate in the production process of wood-plastic composite material products at present and use toxic chemical (as Benzyl Chloride), and plasticizing product needs to use a large amount of water and ethanol to clean, and causes the secondary pollution of environment, or adopt high speed machine means (as high-speed mixing, mechanical activation), mechanical wear and energy consumption larger, or Financial cost high (the clean quick-fried enzymolysis processing again of vapour), sponge surface active groups and chemical reagent is utilized to carry out graft modification, or utilize enzymolysis to reach to improve fusion object between vegetable fibre and thermoplastics, all can not meet market demand.
Goal of the invention
For the problems referred to above, the invention provides a kind of method applied wood fibre and prepare wood plastic composite, to solve the problem of vegetable fibre and plastics fusion faculty and poor mobile performance in existing wood plastic composite, the present invention is achieved in that
Apply the method that wood plastic composite prepared by wood fibre, it is characterized in that, concrete steps are as follows:
1) dry-matter wood fibre is crushed to 20-80 order, adding nitrogenous fertilizer regulates carbon-nitrogen ratio to be 25-35:1, water ratio is 60-70%, add the biological treatment agent accounting for wood fibre dry weight 0.5-5%, in 40-60 DEG C of temperature bottom fermentation 5-15d, then natural air drying to water ratio is 12-14%, obtains powdery biomass lignocellulosic material;
2) by after powdery biomass lignocellulosic material, coupling agent and antioxidant in mass ratio 100:1-5:1-5 mixing, at 55-85 DEG C of temperature, with the rotating speed mixing 10-30min of 300-500rpm, modified biomass powdery lignocellulosic material is obtained;
3) by after modified biomass powdery lignocellulosic material and plastics in mass ratio 6-13:7-14 mixing, at 160-175 DEG C of temperature, with the speed of 500-800rpm mixing 5-20min;
4) material is put into mill, with at 160-180 DEG C of temperature, with the speed extruding pelletization of 380-750rpm, obtain particle and be wood plastic composite.
Further, in step 3) of the present invention, also add filler, modified biomass powdery lignocellulosic material with add filler mass ratio be 9-13:1-2.
Further, wood fibre described in step 1) of the present invention is one or more in rice husk, stalk, sisal dregs, bagasse or bamboo wood residuum; Described biological treatment agent is one or more in straw decomposing inoculant, compost fermentation agent, cellulose degradation microbial inoculum.
Further, bamboo wood residuum of the present invention is bamboo wood industrial wood waste or bamboo wood logging residue.
Further, nitrogenous fertilizer described in step 1) of the present invention is one or more in urea, diammonium phosphate, sulfuric acid two ammonium, ammonium hydrogen phosphate; Step 2) described coupling agent is one or more in silane coupling agent, titanate coupling agent or maleic anhydride coupling agent; Described oxidation inhibitor is one or more in antioxidant 1010, antioxidant 1076, irgasfos 168 or antioxidant 264.
Further, plastics described in step 3) of the present invention are one or more in polypropylene, polyethylene, polyvinyl chloride or polystyrene.
Further, filler described in step 3) of the present invention is one or more in nano silicon, nano-calcium carbonate or nano kaoline.
Further, grain diameter described in step 4) of the present invention is 1-3mm.
The present invention utilizes sisal dregs, bagasse, rice husk, the natural wooden fibers such as stalk and bamboo wood residuum, by adding biological treatment agent, fermentative processing is carried out under suitable carbon-nitrogen ratio and water ratio, utilize the macromole of microbial action breaks wood fibre, reduce fiber molecule intermolecular forces, fermentative processing is utilized to make sisal dregs, bagasse, rice husk, the rheological of the natural wooden fibers such as stalk and bamboo wood residuum makes moderate progress, wood plastic composite is made by granulation, compared with non-fermentative processing wood plastic composite, its melting index, mobility, hydrophobicity and tensile strength have and significantly improve, the wood plastic composite prepared can utilize plastics forming technology and equipment to develop the Wood Plastics Composite Product of various proterties, whole production process low power consuming, environmental protection, be easy to promote.
Accompanying drawing explanation
Fig. 1 is for being embodiment wood plastic composite section electron-microscope scanning picture;
Fig. 2 be fermentation plasticizing rice husk, rice husk respectively with plastic hybrid material granulation masterbatch surface contact angle figure schematic diagram.
Embodiment
Embodiment 1
(1) 100kg is crushed to 20 object dry-matter rice husks, add the straw decomposing inoculant accounting for rice husk dry weight 5%, adding urea regulates rice husk carbon-nitrogen ratio to be 25:1, then adding water regulates material water ratio to be 60%, at 40-60 DEG C of temperature, fermentative processing 5d is carried out after stirring, material is shakeout on concrete floor, treats that natural air drying is 12-14% to water ratio, obtain powdery biomass lignocellulosic material;
(2) get 100kg dry-matter powdery biomass lignocellulosic material and put into mixing machine, add the silane coupling agent of 1kg and the antioxidant 1010 of 3kg is in the high-speed mixer of 500rpm at rotating speed, control temperature, at 55-85 DEG C of mixing 30min, obtains modified biomass powdery lignocellulosic material;
(3) getting the modified biomass powdery lignocellulosic material of 65kg, the polypropylene of 35kg and 10kg nano silicon adds in mixing machine, is 160-175 DEG C in temperature, and rotating speed is mix 10min under 500rpm, obtains mixture;
(4) finally mixture being transported to temperature is 160-180 DEG C, rotating speed be 380rpm mill in carry out high temperature plasticizing, and extruding pelletization, obtain the particle that particle granula is 1-3mm, namely obtain wood plastic composite.
In specific implementation process, also can use stalk, sisal dregs, bagasse and bamboo wood residuum (bamboo wood industrial wood waste or bamboo wood logging residue) in one or more compositions as lignocellulosic material.
Embodiment 2
(1) 100kg is crushed to 60 object dry-matter sisal dregs, add the compost fermentation agent accounting for rice husk dry weight 2%, adding nitrogenous fertilizer (using urea in the present embodiment) regulates sisal dregs carbon-nitrogen ratio to be 30:1, adding water again regulates material water ratio to be 70%, in 40-60 DEG C of temperature bottom fermentation process 10d after stirring, then shakeout by material on concrete floor, natural air drying is 12-14% to water ratio, obtains powdery biomass lignocellulosic material;
(2) get 100kg dry-matter powdery biomass lignocellulosic material and put into mixing machine, add the silane coupling agent of 5kg and the irgasfos 168 of 1kg is in the high-speed mixer of 300rpm at rotating speed, control temperature, at 55-85 DEG C of mixing 10min, obtains modified biomass powdery lignocellulosic material;
(3) adding in mixing machine by the modified biomass powdery lignocellulosic material of 45kg, the polyvinyl chloride of 55kg and 5kg nano kaoline, is 160-175 DEG C in temperature, and rotating speed is mix 30min under 800rpm, obtains mixture;
(4) mixture being transported to temperature is 160-180 DEG C, rotating speed be 750rpm mill in carry out high temperature plasticizing, and extruding pelletization, obtain the particle of 1-3mm, be wood plastic composite.
In specific implementation process, also can use as nitrogenous fertilizer with any one or more compositions in diammonium phosphate, sulfuric acid two ammonium, ammonium hydrogen phosphate.
Embodiment 3
For the fermentation of research wood fibre affects situation to composite property, the present embodiment is divided into two groups, and experimental group preparation method is:
(1) 80 object 100kg dry-matter stalks will be crushed to, add the cellulose degradation microbial inoculum accounting for rice husk dry weight 0.5%, adding appropriate urea regulates stalk carbon-nitrogen ratio to be 30:1, adding water regulates material water ratio to be 65%, in 40-60 DEG C of temperature bottom fermentation process 15d after stirring, then shakeout by material on concrete floor, natural air drying is 12-14% to water ratio, obtains powdery biomass lignocellulosic material;
(2) get 100kg dry-matter powdery biomass lignocellulosic material and put into mixing machine, add the silane coupling agent of 3kg and the antioxidant 264 of 5kg is in the high-speed mixer of 400rpm at rotating speed, control temperature, at 55-85 DEG C of mixing 20min, obtains modified biomass powdery lignocellulosic material;
(3) adding in mixing machine by the modified biomass powdery lignocellulosic material of 30kg, the polyethylene of 70kg and 3kg nano-calcium carbonate, is 160-175 DEG C in temperature, and rotating speed is mix 30min under 600rpm, obtains mixture; Melt indexer, torque rheometer measure melting index and the rheological property of mixture;
(4) mixture being transported to temperature is 160-180 DEG C, rotating speed be 650rpm mill in carry out high temperature plasticizing, and extruding pelletization is to the particle of 1-3mm, obtains wood plastic composite.
Control group preparation method is:
Be crushed to outside the powdery biomass lignocellulosic material in 80 object dry-matter stalks replacement experimental group step (2) divided by 100kg, other steps are identical with experimental group step (2)-(4).
The wood plastic composite of two groups is carried out section electron-microscope scanning, result as shown in Figure 1, wherein Fig. 1 (a) for control group wood plastic composite section electron-microscope scanning figure, Fig. 1 (b) be test group wood plastic composite section electron-microscope scanning figure; From Fig. 1 (b), the wood fibre of experimental group after fermentative processing and polyethylene pattern close, interface fusion; And obvious boundary can be found out between the wood fibre of non-fermentative processing and polyethylene in Fig. 1 (a), and intersection has obvious space, the wood plastic composite interface fusion that visible fermentative processing wood fibre and plastics are mixed with improves.
Measure two groups of surface of wood-plastic composite material contact angles respectively, surperficial dynamic contact angle measuring method: adopt full-automatic contact angle instrument (OCA40Micro type, Germany) to measure.Be that contact angle test fluid measures the change of wood plastic composite spline surfaces contact angle with water; As shown in Figure 2, as seen from Figure 2, the surface contact angle of test group is greater than control group to result, and prolongation in time, surface contact angle rangeability is also less than control group, and this illustrates after biological treatment agent fermentation, surface of wood-plastic composite material polarity diminishes, and hydrophobicity strengthens.
Performance Detection:
(1) measure melting index and the rheological property of the mixture obtained in above-mentioned two groups of material step (3) respectively with melt indexer, torque rheometer, acquired results is as shown in table 1:
Melt index determination method is with reference to the measuring method of GB3682-2000 " thermoplastics melt mass flow rate and melt volume-flow rate ".
Torque rheology measuring method: be placed in by mixture in torque rheometer is 170 DEG C in temperature, and rotating speed is measure 30min under 60rpm condition;
Stretching strength determination method: measure with reference to GB/T17657-1999 " test methods of evaluating the properties of wood-based panels and surface decorated wood-based panels ", directly detect depositing the batten after room temperature 24h, rate of extension is 10mm/min, repeats, gets arithmetical av as test specimen tensile strength for 3 times;
Table 1 experimental group, control group stalk mix rheological and the melt index properties of rear material with plastics
As shown in Table 1, experimental group (fermented stalk/plastics) mixture fusion time is longer, peak torque and balancing torque are all lower than non-fermented stalk/plastic hybrid material, and melting index improves 47.09%, show fermented stalk mix with plastics after the rheological of material to improve amplitude larger.
(2) being sent into respectively in miniature injection machine by two groups of wood plastic composites, is 700bar pressurize 5s 165 DEG C of overdraft, injection moulding growth 100mm, wide 10mm, the dumbbell shaped batten of thick 2mm, in omnipotent mechanical test aircraft measurements batten tensile strength, measurement result is as shown in table 2:
The tensile strength of table 2 experimental group and control group injection moulding batten and elongation at break
| Sample | Tensile strength/MPa | Elongation at break/% |
| Experimental group | 15.54 | 4.14 |
| Control group | 11.92 | 2.51 |
As shown in Table 2, Novel wood-plastic composite material prepared by experimental group (fermented stalk/plastic hybrid material), product strength is higher than wood plastic composite, and elongation at break improves nearly 1 times, show that stalk is after fermentative processing, Novel wood-plastic composite material interface fusion prepared by itself and plastics compound improves, and effectively improves the mechanical strength of wood plastic composite.
(3) two groups of wood plastic composites that embodiment obtains are become flowerpot type respectively by double-screw injection molding, upper port external diameter 160mm, lower port external diameter 130mm, be highly 140mm, after testing, mould straw flowerpot toughness with the wood that experimental group wood plastic composite is obtained to strengthen, compared with moulding straw flowerpot with control group wood, compressed shape variable improves more than 65%.
(4) add in plastic shaping extrusion equipment respectively by the experimental group wood plastic composite that embodiment obtains, conventionally, obtained wood plastic composite Side fascia, door and window lines or skirting, this wallboard or lines have good dimensional stability.
Above embodiment is only the preferred embodiment of the present invention; be not construed as limiting the scope of the present invention; in specific implementation process; concrete technical parameter in the present invention; as the blending ratio etc. of biological treatment agent consumption, coupling agent consumption, wood fibre and plastics; determined by operator in the interval that can limit according to claim, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should belong to the protection domain of the claims in the present invention.
Claims (8)
1. apply the method that wood plastic composite prepared by wood fibre, it is characterized in that, concrete steps are as follows:
1) dry-matter wood fibre is crushed to 20-80 order, adding nitrogenous fertilizer regulates carbon-nitrogen ratio to be 25-35:1, water ratio is 60-70%, add the biological treatment agent accounting for wood fibre dry weight 0.5-5%, in 40-60 DEG C of temperature bottom fermentation 5-15d, then natural air drying to water ratio is 12-14%, obtains powdery biomass lignocellulosic material;
2) by after powdery biomass lignocellulosic material, coupling agent and antioxidant in mass ratio 100:1-5:1-5 mixing, at 55-85 DEG C of temperature, with the rotating speed mixing 10-30min of 300-500rpm, modified biomass powdery lignocellulosic material is obtained;
3) by after modified biomass powdery lignocellulosic material and plastics in mass ratio 6-13:7-14 mixing, at 160-175 DEG C of temperature, with the speed of 500-800rpm mixing 5-20min;
4) material is put into mill, with at 160-180 DEG C of temperature, with the speed extruding pelletization of 380-750rpm, obtain particle and be wood plastic composite.
2. apply wood fibre according to claim 1 and prepare the method for wood plastic composite, it is characterized in that, in step 3), add filler, modified biomass powdery lignocellulosic material with add filler mass ratio be 9-13:1-2.
3. apply wood fibre according to claim 2 and prepare the method for wood plastic composite, it is characterized in that, wood fibre described in step 1) is one or more in rice husk, stalk, sisal dregs, bagasse or bamboo wood residuum; Described biological treatment agent is one or more in straw decomposing inoculant, compost fermentation agent, cellulose degradation microbial inoculum.
4. apply the method that wood plastic composite prepared by wood fibre according to claim 3, it is characterized in that, described bamboo wood residuum is bamboo wood industrial wood waste or bamboo wood logging residue.
5. prepare the method for wood plastic composite according to the described application wood fibre of one of claim 1-4, it is characterized in that, nitrogenous fertilizer described in step 1) is one or more in urea, diammonium phosphate, sulfuric acid two ammonium, ammonium hydrogen phosphate; Step 2) described coupling agent is one or more in silane coupling agent, titanate coupling agent or maleic anhydride coupling agent; Described oxidation inhibitor is one or more in antioxidant 1010, antioxidant 1076, irgasfos 168 or antioxidant 264.
6. apply wood fibre according to claim 5 and prepare the method for wood plastic composite, it is characterized in that, plastics described in step 3) are one or more in polypropylene, polyethylene, polyvinyl chloride or polystyrene.
7. apply wood fibre according to claim 5 and prepare the method for wood plastic composite, it is characterized in that, filler described in step 3) is one or more in nano silicon, nano-calcium carbonate or nano kaoline.
8. apply the method that wood plastic composite prepared by wood fibre according to claim 5, it is characterized in that, grain diameter described in step 4) is 1-3mm.
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