CN102690442A - Method for preparing cellulose filled composite material - Google Patents
Method for preparing cellulose filled composite material Download PDFInfo
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- CN102690442A CN102690442A CN2012101826895A CN201210182689A CN102690442A CN 102690442 A CN102690442 A CN 102690442A CN 2012101826895 A CN2012101826895 A CN 2012101826895A CN 201210182689 A CN201210182689 A CN 201210182689A CN 102690442 A CN102690442 A CN 102690442A
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Abstract
The invention relates to a method for preparing a cellulose filled composite material and belongs to the technical field of composite material preparation. The method comprises the following steps: weighing 1,000-1,100 weight parts of raw material, namely cellulose; drying for 3 hours until the mass percentage of water is less than 1 percent; weighing 60 to 80 weight parts of polyolefin, 5 to 15 weight parts of coupling agent, 5 to 15 weight parts of lubricating agent, 5 to 15 weight parts of impact resistant modifier and 5 to 15 weight parts of dispersing agent; fully mixing raw materials, and processing by using an extruder; and cooling by using a cooling tank, cutting the material to have the required shape, and drying. The prepared composite material has high mechanical properties and thermoplastic property. The composite material can be used for manufacturing various structural products; and the products have different shapes, such as office supplies, living goods (such as plastic basins, doors and windows and rail fences), crossbeams, bearing building materials, electronic product insulating shells, parts in the automobile industry, and interior decoration parts in the aviation industry.
Description
Technical field
The present invention relates to prepare the method for the matrix material that Mierocrystalline cellulose fills, belong to the Composite Preparation technical field.
Background technology
Traditional structural product is to use steel as seat stool, door and window, division board, fence etc., and wood materials or conventional plastic are like Vilaterm, Vestolen PP 7052, other various polyolefine and blend polyolefine etc.As a rule steel and wood material structural strength high, be widely used, can use and make a lot of family products.But shortcoming is steel to get rusty easily and is easy to the burn into poor plasticity; Plastics are then easy ageing of product, and cost is bigger than higher, resource consumption, environmental facies are bigger to DR.
The present invention is a kind of thermoplastic composite polyolefine material of having of plant cellulose filler that contains.Can be used for compressed moulding, rotation molding, extrusion moulding and injection moulding.This composite products can be widely used in and substitute traditional structural product, such as the tables, chairs and benches of office appliance etc., daily necessities (basin, tank, door and window, fence), electronic product casing, automobile and aircraft industry inside fitting component etc.These structural component require its mechanical property, must meet certain standard like bending property, tensile property, shock strength etc.Therefore, to constantly improve these mechanical propertys of material on the one hand, also will consider some other important factor on the other hand: like working temperature, fire resistance, economic benefit, environmental protection factor etc.
In the past decade, use the technology of lignocellulose filled plastics to obtain significant progress at home and abroad.And cellulose wadding be because its fiber properties can better improve mechanical property, particularly snappiness and the impact resistance of plastic polymer, and therefore this filling technique just progressively is caused concern.Invented the polyolefin plastics that a kind of 5-25% of containing Mierocrystalline cellulose is filled like U.S. Pat 7041716 B2.But because Mierocrystalline cellulose has and the visibly different physicochemical property of xylogen, adding Mierocrystalline cellulose in a large number can increase plastics substrate and cellulosic heterozygosis performance, and following process is as extruding the difficulty of processing with the injection moulding aspect in addition.Thereby big limitations a large amount of uses of Mierocrystalline cellulose in polyolefin matrix.
In sum, how better cellulose-binding and polyolefin plastics have become a problem that is worth discussion.To improve plastics substrate and cellulosic cement properties on the one hand, make it have better mechanical property; The workability of not obvious again reduction plastics on the other hand improves the ratio of Mierocrystalline cellulose packing material as much as possible, and the protection environment that economizes on resources reduces cost.
The present invention studies innovation on this basis, has filled up domestic blank, also than the like product performance of present commercialization the leading greatly and similar products at home and abroad of great lifting, particularly impact resistance has been arranged in the world.
Summary of the invention
This patent has been invented a kind of polymer composite, comprises olefin plastics matrix, cellulose wadding, one or more above grafting coupling agents with high reactivity group, possibly comprise one or more above internal lubricant or external lubricants, possibly comprise one or more impact modifier, also possibly comprise a kind of and more than one dispersion agent etc.Raw material is through the super-dry pre-treatment, and Hybrid Heating is extruded, and is processed into the product that shape is fit to commercial prodn.Can be used for follow-up various compressed mouldings, rotation molding, extrusion moulding and injection moulding.
Polyolefin matrix can be pure crude various polyolefine: like new LDPE (film grade), high density polyethylene(HDPE), linear low density polyethylene, Vestolen PP 7052, ethylene propylene copolymer etc.Also can be impure impure Vilaterm, Vestolen PP 7052 or Vilaterm polypropylene copolymer through recycling.
The Mierocrystalline cellulose wide material sources, it can be various waste and old paper, the press reclaimed waste paper that paper-making industry is recycled; Also can be various natural Mierocrystalline celluloses: like straw, flax, jute etc.Mierocrystalline cellulose must be handled through bake drying through the mechanical workout moulding again.What pay particular attention to is: the thermal destruction that drying temperature and time of drying can not make Mierocrystalline cellulose when drying treatment, take place.Cellulosic usage ratio is 10%-70% in this patent, increases significantly than the highest about 30% filling ratio in the present known patent of invention.
The grafting coupling agent is the high polarity lower melting point additive that contains the overactivity group, is used for the Mierocrystalline cellulose and the hydrophobic polymkeric substance of grafting possess hydrophilic property.It can also improve the adding proportion of Mierocrystalline cellulose in polyolefin matrix when improving mechanical property.In the course of processing, the common usage ratio of coupling agent is 1%-10%.
Lubricant has two kinds of different types usually, i.e. internal lubrication type lubricant and external lubrication type lubricant.Internal lubricant is the fluidizer of half lysotype, significantly reduces the plastics viscosity that macro manifestations is come out in the course of processing through the consistency of improving between the inner different micelles of material, to reduce the difficulty of the course of processing., polymer esterification thing saponified, amides, lipid acid etc. like polyethylene wax, OPE, paraffin, metal.And exterior lubricant is to reduce the plastic processing difficulty through lubricious polymeric thing and processor metallic surface, like Fatty Alcohol(C12-C14 and C12-C18), low ester class, ethyl vinyl acetic monomer etc.The main internal lubricant that uses among the present invention, massfraction is 0.5%-10%, also can contain a certain proportion of exterior lubricant.
Impact resistance is a very important mechanical property of matrix material.Some material such as rubber have very high impact strength, but many high performance materials often show very low shock-resistance when low temperature or envrionment temperature.Generally speaking, can improve the impact resistance of plastics through adding some properties-correcting agent.
In addition, this patent also possibly contain some other different types of additive, like dispersion agent, fireproofing agent, stablizer, inhibitor, pigment etc.Also maybe be because the impure a certain proportion of inorganics etc. that contains of raw material.
What this patent was invented is a kind of matrix material that contains the organic cellulose weighting material of external phase thermoplastic polyolefin hydrocarbon substrate and discontinuous phase.The disperse phase that comprises in the matrix material is dispersed in the polyolefin matrix with ultra-fine fibre or particle more uniformly, and its dispersive state with the naked eye is difficult to observation.The disperse phase Mierocrystalline cellulose also possibly comprise particulate state, sheet, plate dress, thread ribbon, cotton-shaped or other shape composition forms.
The polyolefin matrix of external phase can be Vilaterm, Vestolen PP 7052, other polyolefine or the olefin copolymer etc. of any kind.C711-RNA propylene copolymer, the LDPE 1965T of Sabic company and Lupolen 1800U new LDPE (film grade), FPC 100 Vestolen PP 7052 that Lyondellbasel company provides that Flexirene MT 40A linear low density polyethylene, Eraclene MS 80 high density polyethylene(HDPE)s, the Dow company that provides like Eni company produces.Also can be through the impure Vilaterm that contains pigment and other impurity recycling,, other Vestolen PP 7052, other polyolefine or olefin copolymer.Produce the PPC Renenerat olefin copolymer of recycling like Rotho company oneself, Regranulat PP random reclaims Vestolen PP 7052.Polyolefin matrix mass ratio in matrix material is 30%-90%.
The cellulosic filler of discontinuous phase possibly contain various coarse relatively shapes, like sheet, wire, thread, and cotton-shaped, bulk, ribbon shape, bigger particulate state and various non-homogeneous shape.Mierocrystalline cellulose as packing material may reside in much natural or the non-natural raw material.Contain cellulosic natural fiber, like Caulis Sacchari sinensis fiber, flax, jute, hemp, sisal hemp, cotton, ramie, coir, straw, bamboo etc.The Mierocrystalline cellulose source also can be the sub product in the various industrial production lives, like a large amount of paper rubbish etc. of discarding of paper-making industry, old and useless newspaper, books, printing industry generation.Mierocrystalline cellulose shape through processing is having aspect size, long-width ratio, the form etc. various appearances to show, such as bulk, pie, powdery, sheet, cotton-shaped, particulate state etc.Mierocrystalline cellulose and polyolefin matrix can bind in very wide scope.According to the difference of end-use, the ratio of Mierocrystalline cellulose and polyolefin matrix may be different.Mass ratio can change arbitrarily between from 10% to 70%.Because Mierocrystalline cellulose has very strong hydrophilicity, can absorb the central moisture of air, have suitable moisture content.Compound extruding adds man-hour these moisture and can bring difficulty very big in the processing, must carry out dry pre-treatment; But, therefore must take all factors into consideration the temperature and time of drying treatment owing to the at high temperature long-time degraded easily of Mierocrystalline cellulose sex change.In circulation dryer, cellulosic drying temperature needs between 40 ℃-120 ℃, the time between 30 minutes to 12 hours for well.Between 60 ℃-100 ℃ and 1 hour to 6 hours is good.
Coupling agent has played crucial effects, can improve the mechanical property of composite plastic greatly.Effective coupling agent that the present invention uses comprises a kind of polyolefin-wax of maleic anhydride modified modification at least, and concrete to select according to the polyolefin matrix of finally selecting for use be foundation.For example: the metallocene polyethylene wax Licocene PE MA4351 of maleic anhydride modified contains the high grafting property group up to 6%; Maleic anhydride modified Vestolen PP 7052 metallocenes wax Licocene PP MA6452 TP; Maleic anhydride modified Poly Propylene Wax Licocene PP MA 7452; The linear low density polyethylene wax of maleic anhydride modified; The high density polyethylene waxes Bondyram4108 of maleic anhydride modified and Bondyram 5101; Styrene-ethylene/the butylene of maleic anhydride modified-benzene butylene copolymerization wax (SEBS) Kraton FG 1901X; The Poly Propylene Wax Orevac CA100 of maleic anhydride modified etc.Polyolefin-wax through the senior property maleic anhydride of modification contains the high reactivity anhydride group, it its can be fully with the chemical bond of hydrophilic cellulose and hydrophobic polyolefine graft reaction Cheng Xin.
To select needed coupling agent according to the polyolefin matrix in the plastics during use.If Vilaterm is a matrix, because of this selects the modified polyethylene wax coupling agent for use, if matrix is that then should to select modified polypropylene waxes for use be coupling agent to Vestolen PP 7052.For example, the polyethylene wax of toxilic acid anhydridization can significantly improve the vinyon mechanical property that Mierocrystalline cellulose is filled.Anhydride group the effect here is the same with the alcohol acid group, at this activated cellulose strong chemical bond new with formation.Coupling agent can significantly improve the mechanical property of plastics, particularly impact resistance, unit elongation and Young's modulus etc.The coupling agent adding proportion does not wait from 0.5%-20%, preferably is advisable between 1%-10%.
Lubricant can improve the part mechanical property of product, significantly reduces the technology difficulty of the course of processing, strengthens product aesthetic property etc.During actual the use, need the different lubricant of type.The difference according to mechanism of lubricant can be divided into internal lubricant and exterior lubricant.Internal lubricant is compatible with polymkeric substance to a great extent, and it can be reduced friction and give birth to hot, lower melt viscosity, improve flow characteristics.Exterior lubricant then can be improved friction, the reduction tonnage of gloss, minimizing and processor metallic surface.This patent can employable lubricant be to comprise a kind of or more than one the polyolefin-wax exterior lubricant through the maleic anhydride modification, internal lubricant or two kinds of dual-purposes.For example: the Poly Propylene Wax Licocene PP 1602 of the nonpolar lubricant L icowax PED of oxidation state polyethylene wax polar lubricant Licolub H2, oxidation state polyethylene wax 521, N-N ' stearic bicine diester quadrol wax Licowax C, nonpolar unbodied propylene and ethylene copolymerization wax Licocene PP 1302, the Poly Propylene Wax Licocene PP 6102 of nonpolar crystal form, nonpolar amorphous state.Special needs to be pointed out is: when doing lubricant,, can add coupling agent because itself have the character of coupling agent with the mixture Struktol TPW 104 of fatty acid group metal carboxylate and acid amides or diamide.The lubricant adding proportion does not wait from 0.5%-20%, preferably is advisable between 1%-10%.
The present invention possibly use one or more impact modifier.The coupling agent Licocene PP MA 7452 that before mentioned, Licocene PP MA 6452 TP, Licocene PE MA 4351 etc.; Also have lubricant as indicated above such as Licocene PP 6102, Licocene PP 1302 etc., these additives can use as coupling agent and can use as impact modifier again.It should be noted that: the anti-impact modifier Bondyram 7103 that uses MALEIC ANHYDRIDE with high workability to change, can not add the additive of strongly-acid and oxidisability simultaneously.The impact modifier adding proportion does not wait from 0.5%-20%, preferably is advisable between 0.5%-10%.
In addition, the present invention also possibly use one or more dispersion agent, improves the dispersing property of Mierocrystalline cellulose in polyolefin matrix, makes it more even, thereby reduces the defective of product.For example, make dispersant B YK P-4102 can disperse to be adsorbed on the filling surface, in the course of processing, help filler and extrude better the dispersion, use modified fat acid Struktol TPW 113 can better wetting and dispersion filler.The dispersion agent adding proportion does not wait from 0.5%-20%, preferably is advisable between 0.5%-10%.
This patent plastics possibly also contain some other additive, like stablizer, inhibitor, pigment, fire-retardant material etc.All additive total amounts can not surpass 20%, are the best to be no more than 10%.Because the cellulosic material source is various, possibly also contain some inorganic fillers, like clay, lime carbonate, kaolin etc., the 0.5%-20% that inorganic content accounts for total amount does not wait, and concrete content depends on the purity of Mierocrystalline cellulose packing material.
Extrude in the model at twin screw, all raw materials all must keep dry, and add forcing machine then simultaneously and process.Extrusion condition is relevant with plastics substrate, must be between 130 ℃-180 ℃ such as the PEM temperature, and polypropylene-base suggestion temperature is controlled between 150 ℃-200 ℃.Its fusing point of all additives must be lower than processing temperature, and person's additive is not difficult to uniform mixing and produces due effect.What pay particular attention to is: the temperature of twin screw extruder work selects also will consider cellulosic degradation temperature that in normal range of operation, it is low more good more that temperature is selected.What prevent cellulose degradation can also use the side charging, promptly adds all raw materials except that Mierocrystalline cellulose earlier, uses side feed system feeding at the forcing machine middle part.Be machined into the different final plastic prod of different shape after the extrusion moulding.
Composite plastic carries out the product that various needs are produced in further compressed moulding, rotation molding, extrusion moulding and injection moulding, particularly functional product.As: plastic tub, plastics casing, component, refuse container, seat stool, fence, hollow makes up, sheet material etc.Can be used for material of construction, small stores, office appliance, automobile component, aircraft industry inner components etc.
The present invention can be used for making various structural products.On these product appearances various shape can be arranged, like office appliance (tables, chairs and benches), daily necessities such as plastic tub, door and window, fence, crossbeam, load-bearing building materials, electronic product insulated shell, automotive industry component, aircraft industry inside fitting component etc.This material contains recovery product, old and useless newspaper, recycling Mierocrystalline cellulose or natural cellulose that paper-making industry produces, polymkeric substance, additive, pigment etc.What need particularly point out is that the present invention has improved the processability of Mierocrystalline cellulose filled plastics, makes it be easier to process like compressed moulding, rotation molding, extrusion moulding and injection moulding etc., can manufacture and design the plastic prod of random shape.
With at present domestic and international compared with techniques, the advantage that the present invention gives prominence to is:
1) the cellulose wadding wide material sources are cheap.Insensitive to Mierocrystalline cellulose purity, wide impurity scope can be arranged.The usage ratio of packing material is much higher than the 5-20% in the present commercial product in plastics, has reached surprising 10%-70%, has greatly reduced the production cost of plastics.
2) compare with up-to-date research both at home and abroad, the present invention has promoted the impact resistance of plastics, mechanical propertys such as ductility significantly.Impact resistance particularly, the progress up-to-date with European Union is more than doubled on year-on-year basis.
3) the additive relative low price of using, the additive source is present well-known in the world chemical company provides steady sources to be easy to get, easy to use.
4) greatly reduce the usage ratio of pure plastics, the plastics source can be fresh crude, also can recycle.Help to reduce cost, economize on resources, protect environment.
5) end-use is extensive, can be used for material of construction, small stores, office appliance, automobile component, electronic product insulated shell, aircraft industry inner components etc.Has high commercial application prospect.
Description of drawings
The SEM figure that Fig. 1 obtains for combining embodiment one.
The extruded product particle of Fig. 2 for combining embodiment 2 to obtain.
Embodiment
Below in conjunction with scheme the present invention is elaborated:
Embodiment 1
Take by weighing disregard message paper scrap 1000 grams that Creafloc Pellitized recycles through prilling processing.It is the old and useless newspaper that reclaims, and staple is a Mierocrystalline cellulose, and TGA analyzes and shows that it contains mass ratio is 6.7% moisture, and mass ratio is 20.1% inorganics residue, possibly be lime carbonate, kaolin, clay etc.It was added in loft drier 3 hours, record its moisture mass ratio less than 1%.Take by weighing Flexirene MT 40A linear low density polyethylene 700 grams, Licocene PE MA 4351 Vilaterm coupling agents 100 grams, Licolub H12 internal lubricant 100 grams, Bondyram 7103 impact modifier 100 grams again.After the thorough mixing, add twin screw extruder processing together, processing temperature is controlled at 180 ℃.After the extrusion moulding, with the cooling of cooling mortise, cut mechanically becomes particulate state then, and particle can carry out injection moulding processing after super-dry, and Fig. 1 extrudes the batten section picture of matrix material under SEM of processing with injection moulding with scheme 1 corresponding experiment B9 through twin screw.The actual specification that records is 170mm * 10mm * 4mm sample strip percentage of elongation 5.8%, impact resistance 26.86 (kJ/m
2).As the result of the product on the market of reference under on year-on-year basis: Fibrolon P8540 extensibility is 2.85%, and impact resistance is 10.39 (kJ/m
2); Woodfiber Inject 183 extensibilitys 3.37%, impact resistance 12.74 (kJ/m
2).Considerably beyond the existing market performance of products more than one times.
The SEM figure that Fig. 1 obtains for combining embodiment one.
Embodiment 2
Take by weighing F2 raw material 1000 grams, the source is that the mixture of old and useless newspaper and sawmilling is processed through the deinking bleaching.Its water cut mass ratio that uses TGA to survey is 8.3%, and the inorganic content mass ratio is 17.3%.Put it in the vacuum drier dry 3 hours, its moisture content mass ratio of survey is less than 1%.Take by weighing PP FPC 100 PP GRANULESs 700 grams again, Licocene PP MA 6452 TP Poly Propylene Wax coupling agents 100 grams, Poly Propylene Wax lubricant L icocene PP 1302 is totally 100 grams.Except that F2, all the other all raw materials add twin screw extruder, and extrusion temperature is controlled at about 200 ℃.F2 is put into the side feed system of twin screw extruder.When treating that forcing machine is normally extruded, the product cooling is cut into particulate state, carry out injection moulding after the drying.The actual specification that records is that 170mm * 10mm * 4mm sample strip is drawn percentage of elongation 5.7%, impact resistance 28.34 (kJ/m
2), also to promote to some extent than instance 1 performance.
The extruded product particle of Fig. 2 for combining embodiment 2 to obtain.
Claims (10)
1. the method for the preparation Mierocrystalline cellulose matrix material of filling is characterized in that this method has following technological process: take by weighing that to contain staple be cellulosic raw material 1000-1100 part weight; It is carried out dry pre-treatment 3 hours, record its moisture mass percent less than 1%; Taking by weighing the polyolefine raw material again is 60-80 part weight, coupling agent 5-15 part weight, lubricant 5-15 part weight, impact modifier 5-15 part weight, dispersion agent 5-15 part weight; After the raw material thorough mixing, add forcing machine processing together; After the extrusion moulding, with the cooling of cooling mortise, cut mechanically becomes the desired shape after drying.
2. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that described Mierocrystalline cellulose is natural Mierocrystalline cellulose, is Caulis Sacchari sinensis fiber, flax, jute, hemp, sisal hemp, cotton, ramie, coir, straw or bamboo; Perhaps be the cellulose sub product in the industrial production life, be a large amount of discarded paper rubbish that paper-making industry, old and useless newspaper, books or printing industry produce; Cellulosic pre-treatment drying temperature is between 40-120 ℃, and the time is 30-12 hour; Be advisable with 1-6 hour with 60-100 ℃; Mierocrystalline cellulose functional quality per-cent is 10%-70%.
3. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled; It is characterized in that described polyolefin matrix can be pure crude various polyolefine, is new LDPE (film grade), high density polyethylene(HDPE), linear low density polyethylene, Vestolen PP 7052, other polymkeric substance or other multipolymers; Also can be impure impure Vilaterm, Vestolen PP 7052, other polymkeric substance or other multipolymers through recycling; The polyolefine mass percent is 30%-90%.
4. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that using the polyolefin-wax coupling agent that comprises a kind of maleic anhydride modified modification at least; The selection of coupling agent is foundation according to the polyolefin matrix that uses; It is 0.5%-20% that coupling agent adds mass percent, preferably is advisable between 1%-10%.
5. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that using and contains one or more at least through the lubricant after the maleic anhydride modified modification; It is 0.5%-20% that lubricant adds mass percent, is advisable with 1%-10%.
6. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that using impact modifier; The impact modifier mass percent is 0.5%-20%, is advisable with 0.5%-10%.
7. the method for preparing the Mierocrystalline cellulose filled composite materials as claimed in claim 1 is characterized in that using dispersion agent; It is 0.5%-20% that dispersion agent adds mass percent, is advisable with 0.5%-10%.
8. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that using some other additive, and these additives are one or more in stablizer, inhibitor, pigment or the fire-retardant material; All additive mass percents can not surpass 20%, are advisable to be no more than 10%.
9. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that also can containing some inorganic fillers, and these inorganic fillers are one or more in clay, lime carbonate or the kaolin; Inorganics quality per-cent accounts for the 0.5%-20% of total amount.
10. the method for the matrix material that preparation Mierocrystalline cellulose as claimed in claim 1 is filled is characterized in that the PEM processing temperature must be between 130-180 ℃, and the polypropylene-base processing temperature is controlled between 150-200 ℃.
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CN103342786A (en) * | 2013-06-14 | 2013-10-09 | 中南民族大学 | Bagasse/polyethylene composite material and preparation method thereof |
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