CN102408736B - Flame retardant high-wood content wood-plastic composite material and preparation method thereof - Google Patents
Flame retardant high-wood content wood-plastic composite material and preparation method thereof Download PDFInfo
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Abstract
A flame retardant high-wood content wood-plastic composite material and a preparation method thereof relate to a wood-plastic composite material and a preparation method thereof, wherein the problem of easy burning of the wood-plastic composite material with high wood content and the problems of high fire retardant addition amount, low anti-flaming efficiency and high cost of the existing flame retardant treatment technology are solved. The material is prepared from a fire retardant for wood fibers, a wood fiber material, thermoplastic plastics, a fire retardant for plastics, a coupling agent, a lubricant, an antioxidant, a smoke eliminating agent and auxiliaries. The method comprises the following steps of: weighing raw materials; preparing a flame retardant processing fluid; preparing a flame retardant wood fiber material; performing melting granulation on the thermoplastic plastics and the fire retardant for plastics to obtain flame retardant thermoplastic plastic base particles; mixing the flame wood fiber material with the flame retardant thermoplastic plastic base particles, the coupling agent, the lubricant, the antioxidant, the smoke eliminating agent and the auxiliaries, thereby obtaining a premix; performing melting compounding on the premix to obtain a melt material; and molding the melt material to obtain the flame retardant high-wood content wood-plastic composite material. The dosage of the fire retardant in the flame retardant high-wood content wood-plastic composite material is low; and the flame retardant high-wood content wood-plastic composite material is high in flame retardant efficiency and low in cost.
Description
Technical field
The present invention relates to wood plastic composite and preparation method thereof.
Background technology
Wood plastic composite is a class with timber or other lignocellulosic material as filling or strongthener, is matrix with the thermoplastic polymer, through a kind of advanced composite material that melt extrudes or technology such as injection molding is made.Compare with traditional wood materials, advantages such as that wood plastic composite has is water-fast, corrosion-resistant, ageing-resistant, anti-ly damage by worms, dimensional stability is good, simultaneously can carry out secondary processing and recycling, help alleviating the timber resources pressure, solve the plastic pollution problem.At present, being applied to automobile inside plaque, construction and decoration, freight pallet, open-air tables and chairs, wrapping material, sleeper, furniture and war industry, is a kind of green material that has development prospect.
Along with the rapid expansion with industry size of improving constantly of wood plastic composite production technology, its application in fields such as upholstery, door and window, floor, furniture, automotive trims constantly increases.In order to improve surperficial woodiness touch and to reduce production costs, the wood plastic composite of actual production is pursued higher wood fibre addition as far as possible, reduces the consumption of plastics.Yet, as the matrix material of mainly being made up of lignocellulosic material and two kinds of combustible matls of plastics, wood plastic composite has the characteristics more inflammable and higher than combustion of wood calorific value than plastics, and fire hazard is very big, fire hazard can not be ignored, and fire-retardant finish is extremely important.
At present, adopt the mode of in wood plastic composite, adding various fire retardants to improve its flame retardant properties more.Though halogen containing flame-retardant can be obtained the good flame effect, but can produce corrodibility and toxic products such as hydrogen halide during this fire retardant material burning, improved fire hazard greatly, can not satisfy environmental requirement, therefore, adopt Halogen, nontoxic, non-corrosive fire retardant prepares flame-retardant wood-plastic composite becomes inexorable trend.Name be called " flame-retardant wood-plastic composite and preparation method thereof (and China Patent No.: ZL200910072237.X; the applying date: in " the patent a kind of flame-retardant wood-plastic composite and preparation method thereof is disclosed on June 10th, 2009), the fire retardant that is adopted be based on melamine pyrophosphate salt or polyphosphoric acid melamine salt, with starch be assist char-forming agent,
Molecular sieve is that synergist, zinc borate are for pressing down the expansion type flame-retarding system that fumicants constitutes; Name is called " flame-proof smoke-inhibiting wood-plastic composite material (China Patent No.: ZL200710072794.2; the applying date: on September 12nd, 2007) disclose a kind of flame-proof smoke-inhibiting wood-plastic composite material in " the patent, the expansion type flame retardant that is adopted is that 20: 1～8 ammonium polyphosphate and starch are formed by weight ratio, and the plastics that adopted are polystyrene and/or the polyvinyl chloride that has added thermo-stabilizer; Name is called " flame-resistant plastic-wood composite materials and preparation method thereof (China Patent No.: ZL200610039985.4; the applying date: on April 28th, 2006) disclose a kind of flame-resistant plastic-wood composite materials and preparation method thereof in " the patent, the expansion type flame retardant that employing is made up of main body ammonium polyphosphate flame retardant, whipping agent and char-forming agent prepares flame-retardant wood-plastic composite material, these methods can obtain flame retardant properties preferably, but need the ammonium polyphosphate amount of adding bigger, this has not only increased the matrix material cost but also its mechanical property has been had disadvantageous effect.In addition, name is called " organic silicon-boron flame-retardant wood-plastic composite material and preparation method thereof (application number: 201010148882.8; applying date: on April 16th, 2010) adopt the plastic matrix contain the boron silicone grafted polymers and vegetable fibre powder and other auxiliary agent blend to prepare organic silicon-boron flame-retardant wood-plastic composite material in " the patent, though keep mechanical property preferably, the material flame retardant effect is not good enough; Name is called " a kind of flame-retardant wood-plastic composite material and preparation method thereof (application number: 201010288686.0; applying date: on September 21st, 2010) adopt alkali lye, alcoholic solution and trimeric cyanamide saturated hot-water solution-treated to obtain modified wood powder in " the patent, carry out the compound preparation flame-retardant wood-plastic composite material of fusion with hydrated metal oxide, polymeric matrix, treatment process is comparatively complicated.
" forest-science " Song Yongming etc., the 47th the 7th phase of volume, the 145-150 page or leaf, disclose the method for preparing wood plastic composite in " expansible black lead and ammonium polyphosphate are to the cooperative flame retardant effect of wood powder/polypropylene composite material " of in July, 2011 record, the fire retardant addition is big, flame retarding efficiency is not high, cost is bigger than normal and the problem of poor mechanical property but exist.
On the whole, prior art is primarily aimed at polymeric matrix, realizes needing fire-retardant finish to matrix material to add a large amount of fire retardants and obtain flame retardant effect preferably by adding mode that acid source and char-forming agent constitute the expansion type flame-retarding system, this causes cost to increase, and flame retarding efficiency is not high.
Summary of the invention
The present invention seeks to be easy to burn and existing fire-retardant finish technology exists that the fire retardant addition is big, flame retarding efficiency is not high, cost is bigger than normal and the problem of poor mechanical property, and high wooden content wood plastic composite of a kind of flame retardant type and preparation method thereof is provided for the wood plastic composite that solves high wooden content.
The high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part but the auxiliary agent of fumicants and 0～5 part make; Wherein the wood fibre fire retardant is phosphoric acid guanylurea, fire retardant FR W, methylolation phosphoric acid guanylurea, ammonium polyphosphate, ammonium pyrophosphate, ammonium hydrogen phosphate, primary ammonium phosphate, ammonium sulfate, trimeric cyanamide or melamine pyrophosphate; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is high-polymerization degree ammonium polyphosphate, red phosphorus, expansible black lead, melamine cyanurate or phosphoric acid ester; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder.
The preparation method of the high wooden content wood plastic composite of flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part the auxiliary agent that presses down fumicants and 0～5 part; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 0.5%～3% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50～100r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 5～20min under 70～120 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30～50r/min carries out fusion, obtains melt material; Seven, melt material is by extruding, promptly obtaining the high wooden content wood plastic composite of flame retardant type after injection moulding, hot pressing or the compression molding; Wherein the wood fibre fire retardant is phosphoric acid guanylurea, fire retardant FR W, methylolation phosphoric acid guanylurea, ammonium polyphosphate, ammonium pyrophosphate, ammonium hydrogen phosphate, primary ammonium phosphate, ammonium sulfate, trimeric cyanamide or melamine pyrophosphate in the step 1; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is high-polymerization degree ammonium polyphosphate, red phosphorus, expansible black lead, melamine cyanurate or phosphoric acid ester; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder; Wood fibre with fire retardant and water is according to ratio of weight and number 5～25 in the step 2: 125～175 mix.
The present invention adopts polyolefin plastics to prepare wood plastic composite as matrix, make full use of its wide material sources, be easy to advantages such as forming process, carry out fire-retardant to lignocellulosic material and thermoplastics respectively by adding different fire retardants to obtain cooperative flame retardant effect preferably, make full use of the one-tenth charcoal effect of lignocellulosic material itself, reduce the fire retardant consumption, give the wood plastic composite good flame retardancy, make that the Application Areas of wood plastic composite obtains expanding, can be widely used in indoor and the flame retardant properties public place that has certain requirements.
Because lignocellulosic material mainly is made up of Mierocrystalline cellulose, hemicellulose and xylogen, it itself is the many carbon superpolymer that contains a large amount of alcoholic extract hydroxyl groups and phenolic hydroxyl group, has good carbon-forming performance, therefore for the wood plastic composite of the wooden content of height, can utilize wood fibre to become charcoal, cooperate plastics to constitute the expansion type flame-retarding system to realize fire-retardant to wood plastic composite with fire retardant with fire retardant catalysis wood fibre, not only do not need additionally to add char-forming agent, and the fire retardant consumption is few, the flame retarding efficiency height, technology is simple, and cost is low.
The high wooden content wood plastic composite of the flame retardant type of the present invention's preparation not only has fire-retardant preferably and smoke suppressing, and kept its original imitative wood effect and mechanical property preferably, can be widely used in fields such as building decoration, furniture manufacturing, interior decoration, automotive trim and door-window section bar.
Embodiment
Embodiment one: the high wooden content wood plastic composite of present embodiment flame retardant type by ratio of weight and the number of copies by 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part but the auxiliary agent of fumicants and 0～5 part make; Wherein the wood fibre fire retardant is phosphoric acid guanylurea, fire retardant FR W, methylolation phosphoric acid guanylurea, ammonium polyphosphate, ammonium pyrophosphate, ammonium hydrogen phosphate, primary ammonium phosphate, ammonium sulfate, trimeric cyanamide or melamine pyrophosphate; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is high-polymerization degree ammonium polyphosphate, red phosphorus, expansible black lead, melamine cyanurate or phosphoric acid ester; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder.
Press when lignocellulosic material is formed for two or more material in the present embodiment arbitrarily than mixing; When forming for two or more material, presses thermoplastics arbitrarily than mixing; When forming for two or more material, presses the plastics fire retardant arbitrarily than mixing; When forming for two or more material, presses by coupling agent arbitrarily than mixing; When forming for two or more material, presses lubricant arbitrarily than mixing; When forming for two or more material, presses by oxidation inhibitor arbitrarily than mixing; Press down when fumicants is formed for two or more material and press arbitrarily than mixing.
Embodiment two: present embodiment and embodiment one are different be the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 5 parts wood fibre with fire retardant, 50 parts lignocellulosic material, 50 parts thermoplastics, 5 parts plastics with fire retardant, 2 parts coupling agent, 1 part lubricant, 0.1 part oxidation inhibitor and 1 part but fumicants make.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different be the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 25 parts wood fibre with fire retardant, 70 parts lignocellulosic material, 30 parts thermoplastics, 25 parts plastics with fire retardant, 8 parts coupling agent, 3 parts lubricant, 3 parts oxidation inhibitor, 5 parts but the auxiliary agent of fumicants and 5 parts make.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different be the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 10～20 parts wood fibre with fire retardant, 55～65 parts lignocellulosic material, 35～45 parts thermoplastics, 10～20 parts plastics with fire retardant, 3～7 parts coupling agent, 1.5～2.5 parts lubricant, 0.5～2 part oxidation inhibitor, 2～4 parts but the auxiliary agent of fumicants and 1～4 part make.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one are different be the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 15 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 15 parts plastics with fire retardant, 5 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor, 3 parts but the auxiliary agent of fumicants and 3 parts make.Other is identical with embodiment one.
Embodiment six: present embodiment is different with one of embodiment one to five is that the particle order number of lignocellulosic material is 10～300 orders.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different with one of embodiment one to five is that the particle order number of lignocellulosic material is 50 orders.Other is identical with one of embodiment one to five.
Embodiment eight: present embodiment is different with one of embodiment one to five is that the particle order number of lignocellulosic material is 100 orders.Other is identical with one of embodiment one to five.
Embodiment nine: present embodiment is different with one of embodiment one to five is that the particle order number of lignocellulosic material is 200 orders.Other is identical with one of embodiment one to five.
Embodiment ten: present embodiment is different with one of embodiment one to nine is that the polymerization degree of high-polymerization degree ammonium polyphosphate is greater than 1000.Other is identical with one of embodiment one to nine.
Embodiment 11: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part the auxiliary agent that presses down fumicants and 0～5 part; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 0.5%～3% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50～100r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 5～20min under 70～120 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30～50r/min carries out fusion, obtains melt material; Seven, melt material is by extruding, promptly obtaining the high wooden content wood plastic composite of flame retardant type after injection moulding, hot pressing or the compression molding; Wherein the wood fibre fire retardant is phosphoric acid guanylurea, fire retardant FR W, methylolation phosphoric acid guanylurea, ammonium polyphosphate, ammonium pyrophosphate, ammonium hydrogen phosphate, primary ammonium phosphate, ammonium sulfate, trimeric cyanamide or melamine pyrophosphate in the step 1; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is high-polymerization degree ammonium polyphosphate, red phosphorus, expansible black lead, melamine cyanurate or phosphoric acid ester; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder; Wood fibre with fire retardant and water is according to ratio of weight and number 5～25 in the step 2: 125～175 mix.
Press when lignocellulosic material is formed for two or more material in the present embodiment step 1 arbitrarily than mixing; When forming for two or more material, presses thermoplastics arbitrarily than mixing; When forming for two or more material, presses the plastics fire retardant arbitrarily than mixing; When forming for two or more material, presses by coupling agent arbitrarily than mixing; When forming for two or more material, presses lubricant arbitrarily than mixing; When forming for two or more material, presses by oxidation inhibitor arbitrarily than mixing; Press down when fumicants is formed for two or more material and press arbitrarily than mixing.
Injection moulding is that melt material is injected die cavity in the present embodiment step 7, obtains molding behind cooling curing.
Embodiment 12: present embodiment and embodiment 11 are different be take by weighing by ratio of weight and the number of copies in the step 1 20 parts wood fibre with fire retardant, 55 parts lignocellulosic material, 45 parts thermoplastics, 20 parts plastics with the fumicants that presses down of fire retardant, 6 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor and 2 parts.Other step and parameter are identical with embodiment 11.
Embodiment 13: present embodiment and embodiment 11 are different be take by weighing by ratio of weight and the number of copies in the step 1 10 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 10 parts plastics with fire retardant, 3 parts coupling agent, 1 part lubricant, 1.5 parts oxidation inhibitor, 3 parts the auxiliary agent that presses down fumicants and 2 parts.Other step and parameter are identical with embodiment 11.
Embodiment 14: present embodiment is different with one of embodiment 11 to 13 is that the particle order number of lignocellulosic material in the step 1 is 10～300 orders.Other is identical with one of embodiment one to five.Other step and parameter are identical with one of embodiment 11 to 13.
Embodiment 15: present embodiment is different with one of embodiment 11 to 14 is that the polymerization degree of high-polymerization degree ammonium polyphosphate in the step 1 is greater than 1000.Other step and parameter are identical with one of embodiment 11 to 14.
Embodiment 16: what present embodiment was different with one of embodiment 11 to 15 is that the water ratio that is dried under 105 ℃ in the step 3 in the material is 0.5%.Other step and parameter are identical with one of embodiment 11 to 15.
Embodiment 17: what present embodiment was different with one of embodiment 11 to 15 is that the water ratio that is dried under 105 ℃ in the step 3 in the material is 3%.Other step and parameter are identical with one of embodiment 11 to 15.
Embodiment 18: what present embodiment was different with one of embodiment 11 to 15 is that the water ratio that is dried under 105 ℃ in the step 3 in the material is 1%.Other step and parameter are identical with one of embodiment 11 to 15.
Embodiment 19: present embodiment is different with one of embodiment 11 to 18 is that in the step 4 thermoplastics that takes by weighing and plastics to be placed temperature with fire retardant be that 140～180 ℃, screw speed are that the twin screw extruder of 100r/min carries out melt pelletization.Other step and parameter are identical with one of embodiment 11 to 18.
Embodiment 20: present embodiment is different with one of embodiment 11 to 18 is that in the step 4 thermoplastics that takes by weighing and plastics to be placed temperature with fire retardant be that 140～180 ℃, screw speed are that the twin screw extruder of 50r/min carries out melt pelletization.Other step and parameter are identical with one of embodiment 11 to 18.
Embodiment 21: present embodiment is different with one of embodiment 11 to 18 is that in the step 4 thermoplastics that takes by weighing and plastics to be placed temperature with fire retardant be that 140～180 ℃, screw speed are that the twin screw extruder of 80r/min carries out melt pelletization.Other step and parameter are identical with one of embodiment 11 to 18.
Embodiment 22: present embodiment is different with one of embodiment 11 to 21 is to mix 20min in the step 5 under temperature is 70 ℃ condition, obtains Preblend.Other step and parameter are identical with one of embodiment 11 to 21.
Embodiment 23: present embodiment is different with one of embodiment 11 to 21 is to mix 5min in the step 5 under temperature is 120 ℃ condition, obtains Preblend.Other step and parameter are identical with one of embodiment 11 to 21.
Embodiment 24: present embodiment is different with one of embodiment 11 to 21 is to mix 10min in the step 5 under temperature is 100 ℃ condition, obtains Preblend.Other step and parameter are identical with one of embodiment 11 to 21.
Embodiment 25: present embodiment is different with one of embodiment 11 to 24 is that in the step 6 Preblend to be placed temperature to be that 135～170 ℃, screw speed are that the twin screw extruder of 50r/min carries out fusion compound, obtains melt material.Other step and parameter are identical with one of embodiment 11 to 24.
Embodiment 26: present embodiment is different with one of embodiment 11 to 24 is that in the step 6 Preblend to be placed temperature to be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion compound, obtains melt material.Other step and parameter are identical with one of embodiment 11 to 24.
Embodiment 27: present embodiment is different with one of embodiment 11 to 24 is that in the step 6 Preblend to be placed temperature to be that 135～170 ℃, screw speed are that the twin screw extruder of 40r/min carries out fusion compound, obtains melt material.Other step and parameter are identical with one of embodiment 11 to 24.
Embodiment 28: present embodiment is different with one of embodiment 11 to 27 is that to extrude in the step 7 be to adopt conical double screw extruder, parallel double-screw extruder or single screw rod bar forcing machine with the melt material extrusion moulding.Other step and parameter are identical with one of embodiment 11 to 27.
Embodiment 29: present embodiment is different with one of embodiment 11 to 28 is that hot pressing or compression molding are melt material to be placed be hot pressed into sheet material or special-shaped product on the thermocompressor in the step 7.Other step and parameter are identical with one of embodiment 11 to 28.
Embodiment 30: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 6 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 12 parts plastics with the fumicants that presses down of fire retardant, 3 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor and 2 parts; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 2% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 70r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 15min under 80 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion, obtains melt material; Seven, melt material is by promptly obtaining the high wooden content wood plastic composite of flame retardant type after hot-forming; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea in the step 1; Lignocellulosic material is a wood powder; Thermoplastics is a polyethylene; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is the polyethylene of modified by maleic acid anhydride graft; Lubricant is a paraffin; Oxidation inhibitor is antioxidant 1010; Pressing down fumicants is zinc borate; Wood fibre is to mix at 6: 150 according to ratio of weight and number with fire retardant and water in the step 2.
The particle order number of lignocellulosic material is 80～100 orders in the present embodiment step 1.
Hot-forming in the present embodiment step 7 is that melt material is placed on the thermocompressor, is at platen temperature up and down that hot pressing 2～3min forms sheet material under 150～160 ℃ the condition.
It is as shown in table 1 that present embodiment prepares the performance index of the high wooden content wood plastic composite of obtained flame-retardant type, and as seen, mechanical property and flame retardant properties that present embodiment prepares the wooden content wood plastic composite of obtained flame-retardant type height are good.
Table 1
The embodiment hentriaconta-: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 14 parts wood fibre with fire retardant, 70 parts lignocellulosic material, 30 parts thermoplastics, 5 parts plastics with the fumicants that presses down of fire retardant, 3.5 parts coupling agent, 2 parts lubricant, 2 parts oxidation inhibitor and 2 parts; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 2% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 15min under 80 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion, obtains melt material; Seven, melt material is by promptly obtaining the high wooden content wood plastic composite of flame retardant type after hot-forming; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea in the step 1; Lignocellulosic material is a wood powder; Thermoplastics is a polyethylene; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is the polyethylene of modified by maleic acid anhydride graft; Lubricant is the mixture of paraffin and polyethylene wax; Oxidation inhibitor is antioxidant 1010; Pressing down fumicants is zinc borate; Wood fibre is to mix at 14: 175 according to ratio of weight and number with fire retardant and water in the step 2.
Lubricant is that paraffin and polyethylene wax mixed in 1: 1 by volume in the present embodiment step 1.
The particle order number of lignocellulosic material is 80～100 orders in the present embodiment step 1.
Hot-forming in the present embodiment step 7 is that melt material is placed on the thermocompressor, is at platen temperature up and down that hot pressing 2～3min forms sheet material under 150～160 ℃ the condition.
It is as shown in table 2 that present embodiment prepares the performance index of the high wooden content wood plastic composite of obtained flame-retardant type, and as seen, mechanical property and flame retardant properties that present embodiment prepares the wooden content wood plastic composite of obtained flame-retardant type height are good.
Table 2
Embodiment 32: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 12 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 6 parts plastics with fire retardant, 3 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor, 2 parts the auxiliary agent that presses down fumicants and 1 part; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 2% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 10min under 100 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion, obtains melt material; Seven, melt material is by promptly obtaining the high wooden content wood plastic composite of flame retardant type after hot-forming; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea in the step 1; Lignocellulosic material is a wood powder; Thermoplastics is a polypropylene; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is the polypropylene of modified by maleic acid anhydride graft; Lubricant is an oxidized polyethlene wax; Oxidation inhibitor is antioxidant 1076; Pressing down fumicants is magnesium hydroxide; Auxiliary agent is a Paris white; Wood fibre is to mix at 12: 150 according to ratio of weight and number with fire retardant and water in the step 2.
The particle order number of lignocellulosic material is 80～100 orders in the present embodiment step 1.
Hot-forming in the present embodiment step 7 is that melt material is placed on the thermocompressor, is at platen temperature up and down that hot pressing 2～3min forms sheet material under 150～160 ℃ the condition.
It is as shown in table 3 that present embodiment prepares the performance index of the high wooden content wood plastic composite of obtained flame-retardant type, and as seen, mechanical property and flame retardant properties that present embodiment prepares the wooden content wood plastic composite of obtained flame-retardant type height are good.
Table 3
Embodiment 33: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 6 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 12 parts plastics with fire retardant, 3 parts coupling agent, 2 parts lubricant, 1.5 parts oxidation inhibitor, 3 parts the auxiliary agent that presses down fumicants and 2 parts; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 2% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 15min under 80 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion, obtains melt material; Seven, melt material is by promptly obtaining the high wooden content wood plastic composite of flame retardant type after hot-forming; Wherein the wood fibre fire retardant is an ammonium polyphosphate in the step 1; Lignocellulosic material is a straw powder; Thermoplastics is the polyethylene reclaimed materials; The plastics fire retardant is a melamine cyanurate; Coupling agent is the modified by maleic acid anhydride graft polyethylene; Lubricant is a polyethylene wax; Oxidation inhibitor is oxidation inhibitor 1035; Pressing down fumicants is aluminium hydroxide; Auxiliary agent is a talcum powder; Wood fibre is to mix at 6: 150 according to ratio of weight and number with fire retardant and water in the step 2.
The particle order number of lignocellulosic material is 80～100 orders in the present embodiment step 1.
Hot-forming in the present embodiment step 7 is that melt material is placed on the thermocompressor, is at platen temperature up and down that hot pressing 2～3min forms sheet material under 150～160 ℃ the condition.
It is as shown in table 4 that present embodiment prepares the performance index of the high wooden content wood plastic composite of obtained flame-retardant type, and as seen, mechanical property and flame retardant properties that present embodiment prepares the wooden content wood plastic composite of obtained flame-retardant type height are good.
Table 4
Embodiment 34: the preparation method of the high wooden content wood plastic composite of present embodiment flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 9 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 9 parts plastics with fire retardant, 3 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor, 2 parts the auxiliary agent that presses down fumicants and 3 parts; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 2% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 10min under 100 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30r/min carries out fusion, obtains melt material; Seven, melt material is by promptly obtaining the high wooden content wood plastic composite of flame retardant type after hot-forming; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea in the step 1; Lignocellulosic material is a powdered rice hulls; Thermoplastics is a polyethylene; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is the modified by maleic acid anhydride graft polyethylene; Lubricant is a paraffin; Oxidation inhibitor is antioxidant 1010; Pressing down fumicants is zinc borate; Auxiliary agent is a Calucium Silicate powder; Wood fibre is to mix at 9: 150 according to ratio of weight and number with fire retardant and water in the step 2.
The particle order number of lignocellulosic material is 100～120 orders in the present embodiment step 1.
Hot-forming in the present embodiment step 7 is that melt material is placed on the thermocompressor, is at platen temperature up and down that hot pressing 2～3min forms sheet material under 150～160 ℃ the condition.
It is as shown in table 5 that present embodiment prepares the performance index of the high wooden content wood plastic composite of obtained flame-retardant type, and as seen, mechanical property and flame retardant properties that present embodiment prepares the wooden content wood plastic composite of obtained flame-retardant type height are good.
Table 5
Claims (8)
1. the high wooden content wood plastic composite of flame retardant type, it is characterized in that the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part but the auxiliary agent of fumicants and 0～5 part make; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder; Wherein the polymerization degree of high-polymerization degree ammonium polyphosphate is greater than 1000.
2. the high wooden content wood plastic composite of flame retardant type according to claim 1, it is characterized in that the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 10～20 parts wood fibre with fire retardant, 55～65 parts lignocellulosic material, 35～45 parts thermoplastics, 10～20 parts plastics with fire retardant, 3～7 parts coupling agent, 1.5～2.5 parts lubricant, 0.5～2 part oxidation inhibitor, 2～4 parts but the auxiliary agent of fumicants and 1～4 part make.
3. the high wooden content wood plastic composite of flame retardant type according to claim 1, it is characterized in that the high wooden content wood plastic composite of flame retardant type by ratio of weight and the number of copies by 15 parts wood fibre with fire retardant, 60 parts lignocellulosic material, 40 parts thermoplastics, 15 parts plastics with fire retardant, 5 parts coupling agent, 2 parts lubricant, 1 part oxidation inhibitor, 3 parts but the auxiliary agent of fumicants and 3 parts make.
4. according to claim 1, the high wooden content wood plastic composite of 2 or 3 described flame retardant types, it is characterized in that the particle order number of lignocellulosic material is 10～300 orders.
5. the method for preparing the high wooden content wood plastic composite of flame retardant type as claimed in claim 1 is characterized in that the preparation method of the high wooden content wood plastic composite of flame retardant type carries out according to the following steps: one, take by weighing by ratio of weight and the number of copies 5～25 parts wood fibre with fire retardant, 50～70 parts lignocellulosic material, 30～50 parts thermoplastics, 5～25 parts plastics with fire retardant, 2～8 parts coupling agent, 1～3 part lubricant, 0.1～3 part oxidation inhibitor, 1～5 part the auxiliary agent that presses down fumicants and 0～5 part; Two, the wood fibre that takes by weighing is hybridly prepared into fire-retardant treatment liquid with fire retardant and water; Three, the lignocellulosic material that takes by weighing is put in the high-speed mixer, and sprayed fire-retardant treatment liquid on lignocellulosic material, get material, the water ratio that is dried under 105 ℃ in the material is 0.5%～3% then, obtains fire-retardant lignocellulosic material; Four, the thermoplastics that takes by weighing and plastics being placed temperature with fire retardant is that 140～180 ℃, screw speed are that the twin screw extruder of 50～100r/min carries out melt pelletization, obtains flame-proofed thermoplastic plastic substrate particle; Five, with fire-retardant lignocellulosic material, flame-proofed thermoplastic plastic substrate particle, coupling agent, lubricant, oxidation inhibitor, press down fumicants and auxiliary agent is put in the high-speed mixer, be to mix 5～20min under 70～120 ℃ the condition in temperature, obtain Preblend; Six, it is compound Preblend to be placed temperature be that 135～170 ℃, screw speed are that the twin screw extruder of 30～50r/min carries out fusion, obtains melt material; Seven, melt material is by extruding, promptly obtaining the high wooden content wood plastic composite of flame retardant type after injection moulding, hot pressing or the compression molding; Wherein the wood fibre fire retardant is the phosphoric acid guanylurea in the step 1; Lignocellulosic material is one or more the mixture in wood powder, powdered rice hulls, bamboo bits, straw powder, shell powder, bagasse, the flaxen fiber; Thermoplastics is one or more the mixture in polyethylene, polypropylene, polyethylene reclaimed materials or the polypropylene reclaimed materials; The plastics fire retardant is the high-polymerization degree ammonium polyphosphate; Coupling agent is one or more the mixture in the polypropylene of polyethylene, modified by maleic acid anhydride graft of titanic acid ester, aluminic acid ester, isocyanic ester, silane coupling agent, modified by maleic acid anhydride graft; Lubricant is one or more the mixture in paraffin, polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, stearic acid, the Metallic stearates; Oxidation inhibitor is oxidation inhibitor 168, antioxidant 1010, antioxidant 264, antioxidant 1076, antioxidant 2246, oxidation inhibitor 1035, antioxidant 3114, oxidation inhibitor 1790,2, the mixture of one or more in 6-di-tert-butyl-4-methy phenol, tricresyl phosphite (2, the 4-di-tert-butyl-phenyl) ester; Pressing down fumicants is zinc borate, magnesium hydroxide, aluminium hydroxide, molybdic oxide, ammonium octamolybdate, Cu
2The mixture of one or more among the O; Auxiliary agent is Paris white, talcum powder, flyash, carbon black or Calucium Silicate powder; Wood fibre with fire retardant and water is according to ratio of weight and number 5～25 in the step 2: 125～175 mix; The polymerization degree of high-polymerization degree ammonium polyphosphate is greater than 1000.
6. the preparation method of the high wooden content wood plastic composite of flame retardant type according to claim 5 is characterized in that in the step 4 that it is that 140～180 ℃, screw speed are that the twin screw extruder of 80r/min carries out melt pelletization that the thermoplastics that will take by weighing and plastics place temperature with fire retardant.
7. according to the preparation method of claim 5 or the high wooden content wood plastic composite of 6 described flame retardant types, it is characterized in that extruding in the step 7 is to adopt conical double screw extruder, parallel double-screw extruder or single screw rod bar forcing machine with the melt material extrusion moulding.
8. according to the preparation method of claim 5 or the high wooden content wood plastic composite of 6 described flame retardant types, it is characterized in that in the step 7 that hot pressing or compression molding are melt material to be placed be hot pressed into sheet material or special-shaped product on the thermocompressor.
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