CN102850695A - Flame-retardant wood plastic composite based on walnut shell flour and preparation process thereof - Google Patents
Flame-retardant wood plastic composite based on walnut shell flour and preparation process thereof Download PDFInfo
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- CN102850695A CN102850695A CN201210319295XA CN201210319295A CN102850695A CN 102850695 A CN102850695 A CN 102850695A CN 201210319295X A CN201210319295X A CN 201210319295XA CN 201210319295 A CN201210319295 A CN 201210319295A CN 102850695 A CN102850695 A CN 102850695A
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Abstract
The invention provides a flame-retardant wood plastic composite based on walnut shell flour and a preparation process thereof. The composite comprises, by weight, 100 parts of a thermoplastic high polymer resin, 10 to 70 parts of walnut shell flour, 1 to 20 parts of nanometer montmorillonite, 0 to 10 parts of a high polymer modifier, 1 to 6 parts of a surface modifier, 1 to 8 parts of a heat stabilizer, 1 to 5 parts of a lubricant, 1 to 5 parts of a plasticizer and 1 to 5 parts of a composite fire retardant. The preparation process comprises the following steps: drying and crushing walnut shells, carrying out surface chemical modification and wrapping the walnut shell flour with the nanometer montmorillonite; mixing raw materials in a high speed kneader according to a weight ratio as expressed in the above-mentioned formula, carrying out preplasticizing, cooling and fragmenting obtained fused beads and carrying out extrusion molding. The flame-retardant wood plastic composite based on the walnut shell flour provided by the invention has excellent mechanical properties, good weatherability, water resistance, flame retardation, good dimensional stability, resistance to moth and mildew and no heavy metals, formaldehyde and organic volatile matters; and the preparation process is safe, environment-friendly, simple and convenient and has low manufacturing cost.
Description
Technical field
The invention belongs to wood plastic composite and fabricating technology aspect thereof, especially a kind of walnut shell flour flame-retardant wood-plastic composite material and preparation technology thereof.
Background technology
The xylon that adopts in the Wood-plastic material mainly comprises waste wood powder, wood shavings, sawmilling, and vegetable fibre is the rice straw crossed of pulverization process, Pericarppium arachidis hypogaeae, Exocarpium cocois (Cocos nucifera L), sugarcane, flax, pool fiber crops, jute, hemp etc.; Thermoplastics is mainly polyolefine and the PVC such as PE, PP, PS, comprises virgin material, reclaimed materials and the two compound. and xylon and vegetable fibre are initial as Modification material low-cost, that improve the plastics rigidity.Abundant, inexpensive, the light weight of xylon and vegetable fibre source, little to equipment attrition, dimensional stability is good, and electrical insulating property is excellent, and is nontoxic, but reprocessabilty, can biological degradation.
China is as the country of a forest resourceies poorness, and the forest reserves less than is 10 cubic metres per capita, and lumber consumption level less than is 0.22 cubic metre/year per capita, but the wood consumption of China sharply rises, and has to from a large amount of timber of external import.On the other hand, the annual because discarded wood powder amount of wood working remainder of China more than millions of tons, up to ten million tons such as the output of other natural fibers such as rice chaff etc.From this angle, the exploitation of Wood-plastic material will help effective exploitation and utilize these resources, and prospect is very considerable.
According to one's analysis, contain ash content 0.663g, moisture 9.59g, alcohol-benzene extractive 3.71g, xylogen 38.05g, Mierocrystalline cellulose 30.88g, hemicellulose 27.26g in every 100g nut-shell.The past walnut is sold as dry fruit, and its shell is difficult to recycle, and present many walnuts are by deep processing and utilization, and a large amount of nut-shells of concentrating that produce but are dropped or burn, and cause the significant wastage of resource.Therefore, strengthen the comprehensive utilization to nut-shell, avoid the waste of nut-shell resource, the product that the production added value is high not only can effectively be processed solid waste, and can turn waste into wealth, and improves income.
The main component of nut-shell is lignin, Mierocrystalline cellulose and hemicellulose, compares with other plant, and hot water or cold water's extractum, 1%NaOH extractum, acid insoluble lignin content are all higher, and content of cellulose is obviously lower, and many pentosan content and pourous wood are close.
Wood plastic composite refers to utilize waste wood fibre resources and waste plastic resource, the novel environmental friendly materials of making through mixed refining process.This properties of materials integrates the advantage of timber and plastics, the field such as beautifies, the chemical industry ocean is anticorrosion at industrial packaging, outdoor scene and substitutes timber, steel and resin, has unique and purposes widely.The research and development of this technology to the waste resource material utilization, drive processing of agriculture product and for industry and life provide cheap and good-quality novel material significant, this technology also will become an important step in the whole recycling economy.
Although itself has self-extinguishing polyvinyl chloride, in order to improve Drawing abillity, can use in a large number softening agent in the prescription, cause the inflammableness of product to improve.Simultaneously, in order to pursue wood effect and to reduce cost, also can constantly improve wood powder ratio in the wood plastic product, this impact property that not only causes PVC wood to mould sharply descends, and has also aggravated inflammableness and fire hazard that wood is moulded.Produce dense black smoke during burning, can make the people feel to suffocate and the comprehensively decline of ability to see things in their true light, even weak and limp, faintness occurs, until death by suffocation; Smog also enters the scene of fire to the firefighter, rescues fast and brings very large difficulty, has strengthened the destructiveness of fire.As seen, PVC wood is moulded fire-retardant product and must be possessed good smoke suppressing.Therefore, the fire-retardant of PVC wood plastic product and the research that presses down cigarette are caused our very big concern.Smokiness when all burn to macromolecular material in countries in the world has been formulated strict regulation limitations, presses down the prominent position that cigarette has been listed in flame-retarded technology.PVC wood is moulded, and " pressing down cigarette " is more even more important than " fire-retardant ", becomes the matter of utmost importance that must solve.Head it off will make PVC wood mould at cost, energy-conservation, environmental protection, the aspect such as fire-retardant and all produce positive effect.
The objective of the invention is in order to take full advantage of the remaining nut-shell of walnut plantation processing, make intensity height, flame-retardant wood-plastic composite material that cost is low.
Summary of the invention
The present invention is just in order to address the above problem, and provides a kind of flame-retardant wood-plastic composite material based on walnut shell flour and preparation method thereof, the flame-retardant wood-plastic composite material based on walnut shell flour of the present invention, mechanical property is excellent, good weatherability, water-fast, fire-retardant, good stability of the dimension, Anti-moth-eating, mildew-resistant, heavy metal free, formaldehyde and organic volatile, complete processing safety, environmental protection, simple, convenient, cheap for manufacturing cost.
A kind of flame-retardant wood-plastic composite material based on walnut shell flour, the present invention includes walnut shell flour, thermoplastic macromolecule resin and auxiliary agent, wherein auxiliary agent is comprised of nano montmorillonite, macromolecule modifier, surface-modifying agent, thermo-stabilizer, lubricant, softening agent, composite flame-retardant agent; The weight ratio of each component is, the thermoplastic macromolecule resin is 100 parts, walnut shell flour is 10-70 part, nano montmorillonite is 1-20 part, macromolecule modifier is that 0-10 part, surface-modifying agent are 1-6 part, and thermo-stabilizer is that 1-8 part, lubricant are that 1-5 part, softening agent are that 1-5 part, composite flame-retardant agent are 1-5 part.
The water content of walnut shell flour of the present invention is less than 2.5%, and smashing fineness is that 40-120 order and process surface chemical modification are processed; This surface chemical modification is treated to alcohol dissolves surface-modifying agent, and concentration is 5-10%, and is 40-60 ℃ in temperature, and rotating speed is 120-320 rpm, the surface-modifying agent spirituous solution is added in the walnut shell flour disperseed 30-40 minute.
Thermoplastic macromolecule resin of the present invention is selected from single thing in the polyvinyl chloride (PVC) RESINS, polyethylene, polypropylene of polyvinyl chloride (PVC) RESINS, polyethylene, polypropylene or recovery or several mixtures.
Nano montmorillonite of the present invention can be smectite content greater than 80%, and water content is less than 3%, and fineness is 1-8 μ m.
Macromolecule modifier of the present invention can be single thing or the multiple mixture in one or more mixtures of chlorinatedpolyethylene (CPE) or toxilic acid grafted polyethylene or toxilic acid graft polypropylene or polyacrylic ester (ACR) or all acrylic ester class (AIM) or ethylene-vinyl acetate copolymer (EVA) or methyl acrylate-butadiene-styrene ternary graft copolymers (MBS) or acrylonitrile-butadiene-styrene copolymer (ABS) class anti-impact macromolecule modifier.
Surface-modifying agent of the present invention adopts single thing or the multiple mixture in titanate coupling agent or zirconium aluminate or Aluminate or phosphoric acid ester or silane coupling agent or higher fatty acid and salt or nonionic surface active agent or two (2 one hydroxyethyl) methyl tallow based quaternary ammonium salt or octadecyl tribromide ammonium or its chlorinated polypropylene wax and oxidized polyethlene wax or the polyoxyethylene glycol.
Thermo-stabilizer of the present invention is organotin stabilizer or rare-earth stabilizer or lead salt stabilizer, is selected from one or more mixtures in dibutyl tin laurate or two lauric acid dioctyl tins or dialkyl group toxilic acid dibutyl tin or two (Thiovanic acid isooctyl acrylate) dibutyl tin or lauric acid toxilic acid dibutyl tin or tribasic lead sulfate or dibasic lead phosphite or dibasic lead stearate or dibasic lead phthalate or two alkali formula lead phosphates or the lead stearate.
Lubricant of the present invention is one or more mixtures in paraffin or stearic acid or barium stearate or calcium stearate or Zinic stearas or the oxidized polyethlene wax etc.
Softening agent of the present invention is one or more mixtures in Phthalates or aliphatic dibasic acid ester or phosphoric acid ester or polyol ester class or the many esters of gallic acid of benzene or citric acid ester type or polyester or epoxies or the clorafin etc.
Composite flame-retardant agent of the present invention is one or more mixtures in aluminum-magnesium series fire retardant or phosphorus flame retardant or nanoparticle fire retardant or expansion type flame retardant or whisker fire retardant or the ferrocene etc.
A kind of preparation method of the flame-retardant wood-plastic composite material based on walnut shell flour, its manufacturing process is:
(1) nut-shell is pulverized, made fineness reach the 40-120 order, then forced drying makes water content less than 2.5%, and walnut shell flour is carried out surface chemical modification process;
(2) in high-speed mixer, nano montmorillonite is joined in the walnut shell flour after step (1) surface-modifying agent is processed, processed 10-40 minute with 600-900 rpm of high-speed stirring, make the walnut shell flour of nano montmorillonite parcel;
(3) in the high-speed kneading machine, mix than the walnut shell flour with thermoplastic macromolecule resin, macromolecule modifier, thermo-stabilizer, lubricant, softening agent, composite flame-retardant agent and nano montmorillonite parcel by above-mentioned formulation weight, discharging after being 80-90 ℃ to temperature, then in two roller mills in 170-180 ℃ of lower melt blending 2040 minutes.
(4) the gained molten sheet drops into extrusion moulding in the screw extrusion press through cooling off fragmentation.
The invention has the beneficial effects as follows:
(1) opened up extensively the use range of discarded nut-shell, improved the comprehensive utilization degree of nut-shell, namely economized on resources, again protection of the environment.
(2) used wood fibre is walnut shell flour, and the feature of environmental protection of the nut-shell wood plastic composite that makes is more obvious.
(3) can reduce resistance to flow and the nut-shell fiber degradation trend of composite material extrusion moulding process at nut-shell fiber surface clad nano montmorillonite, reach the effect of improving complete processing, improving material property.
(4) owing to added nano montmorillonite, reduce plasticizing viscosity and improved fluidity of molten, reduced energy consumption, improved mechanics and Nai Hou, resistance toheat and the flame retardant resistance of material.
(5) owing to added nano montmorillonite, increase water vapor barrier property and ray barrier, thereby strengthened water tolerance and UV resistant performance.(6) owing to added nano montmorillonite and fire retardant, obviously increase oxygen index and the smoke density grade of wood plastic composite, improved flame retardant properties.
Embodiment
The following examples are only for understanding more easily the present invention, but do not limit the present invention in any way.
EXAMPLE l, embodiment 2, embodiment 3(see Table 1)
Nut-shell is carried out seasoning, make water content less than 8%, with fiber pulverizer nut-shell is pulverized, making fineness is the 60-80 order, and forced drying makes water content less than 2.5%, and carries out the walnut shell flour surface chemical modification and process.In high-speed mixer nano montmorillonite joined in the walnut shell flour of surface modification treatment after good, high-speed stirring was processed 10-40 minutes, made the walnut shell flour of nano montmorillonite parcel; By above-mentioned weight part ratio polyvinyl chloride (PVC) RESINS, macromolecule modifier, thermo-stabilizer, lubricant softening agent, composite flame-retardant agent and modified nano montmorillonite are mixed in the high-speed kneading machine, discharging after being 80-90 ℃ to temperature, then in two roller mills in 170-180 ℃ of lower melt blending 20-40 minutes, the gained molten sheet is broken through the cooling big gun, drops into extrusion moulding (prescription sees Table 1) in the screw extrusion press.Embodiment requires sample preparation, test (the results are shown in Table 2, table 3 and table 4) according to GB.
Embodiment 4 embodiment 5 embodiment 6(see Table 1)
Nut-shell is carried out seasoning, make water content less than 8%, with fiber pulverizer nut-shell is pulverized, making fineness is the 60-80 order, and forced drying makes water content less than 2.5%, and carries out the walnut shell flour surface chemical modification and process.In high-speed mixer nano montmorillonite joined in the walnut shell flour of surface modification treatment after good, high-speed stirring was processed 10-40 minutes, made the walnut shell flour of nano montmorillonite parcel; By above-mentioned weight part ratio polyvinyl resin, macromolecule modifier, lubricant softening agent, composite flame-retardant agent and modified nano montmorillonite are mixed in the high-speed kneading machine, discharging after being 80-90 ℃ to temperature, then in two roller mills in 170-180 ℃ of lower melt blending 2040 minutes, the gained molten sheet is broken through the cooling big gun, drops into extrusion moulding (prescription sees Table 1) in the screw extrusion press.Embodiment requires sample preparation, test (the results are shown in Table 2, table 3 and table 4) according to GB.
Table 1 is based on the prescription (weight amount part) of the flame-retardant wood-plastic composite material of walnut shell flour
Table 2 is based on the quantitative measurement result of the flame-retardant wood-plastic composite material of walnut shell flour
Table 3 is based on the measuring mechanical property result of the flame-retardant wood-plastic composite material of walnut shell flour
Table 4 is based on the flame retardant properties test result of the flame-retardant wood-plastic composite material of walnut shell flour
| Test event | Oxygen index | Smoke density grade |
| Embodiment 1 | 76 | 78 |
| Embodiment 2 | 72 | 76 |
| Embodiment 3 | 67 | 73 |
| Embodiment 4 | 68 | 73 |
| Embodiment 5 | 62 | 72 |
| Embodiment 6 | 53 | 69 |
| Testing standard | GB/T 2406-1993 | GB/T8627-2007 |
Claims (10)
1. flame-retardant wood-plastic composite material based on walnut shell flour, it is characterized in that, comprise walnut shell flour, thermoplastic macromolecule resin and auxiliary agent, wherein auxiliary agent is comprised of nano montmorillonite, macromolecule modifier, surface-modifying agent, thermo-stabilizer, lubricant, softening agent, composite flame-retardant agent; The weight ratio of each component is, the thermoplastic macromolecule resin is 100 parts, walnut shell flour is 10-70 part, nano montmorillonite is 1-20 part, macromolecule modifier is that 0-10 part, surface-modifying agent are 1-6 part, and thermo-stabilizer is that 1-8 part, lubricant are that 1-5 part, softening agent are that 1-5 part, composite flame-retardant agent are 1-5 part.
2. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that, the water content of described walnut shell flour is less than 2.5%, and smashing fineness is that 40-120 order and process surface chemical modification are processed; This surface chemical modification is treated to alcohol dissolves surface-modifying agent, and concentration is 5-10%, and is 40-60 ℃ in temperature, and rotating speed is 120-320 rpm, the surface-modifying agent spirituous solution is added in the walnut shell flour disperseed 30-40 minute.
3. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that, described thermoplastic macromolecule resin is polyvinyl chloride (PVC) RESINS or polyethylene or polyacrylic one or more mixture.
4. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that, described nano montmorillonite be smectite content greater than 80%, water content is less than 3%, fineness is 1-8 μ m; Described macromolecule modifier is one or more mixture of chlorinatedpolyethylene or toxilic acid grafted polyethylene or toxilic acid graft polypropylene or polyacrylic ester or all acrylic ester class or ethylene-vinyl acetate copolymer or methyl acrylate-butadiene-styrene ternary graft copolymers or acrylonitrile-butadiene-styrene copolymer class anti-impact macromolecule modifier.
5. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1, it is characterized in that described surface-modifying agent is one or more the mixture in titanate coupling agent or zirconium aluminate or Aluminate or phosphoric acid ester or silane coupling agent or higher fatty acid and salt or nonionic surface active agent or two methyl tallow based quaternary ammonium salt or octadecyl tribromide ammonium or its chlorinated polypropylene wax or oxidized polyethlene wax or the polyoxyethylene glycol.
6. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that, described thermo-stabilizer is organotin stabilizer or rare-earth stabilizer or hydrotalcite stablizer or lead salt stabilizer; Thermo-stabilizer is one or more mixtures in dibutyl tin laurate or two lauric acid dioctyl tins or dialkyl group toxilic acid dibutyl tin or two (Thiovanic acid isooctyl acrylate) dibutyl tin or lauric acid toxilic acid dibutyl tin, tribasic lead sulfate or dibasic lead phosphite or dibasic lead stearate or dibasic lead phthalate or two alkali formula lead phosphates or the lead stearate.
7. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that, described lubricant is one or more mixture of paraffin or stearic acid or barium stearate or calcium stearate or Zinic stearas or oxidized polyethlene wax.
8. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1, it is characterized in that described softening agent is one or more mixture of Phthalates or aliphatic dibasic acid ester or phosphoric acid ester or polyol ester class or the many esters of gallic acid of benzene or citric acid ester type or polyester or epoxies or clorafin.
9. a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1, it is characterized in that described composite flame-retardant agent is one or more mixtures of aluminum-magnesium series fire retardant or phosphorus flame retardant or nanoparticle fire retardant or expansion type flame retardant or whisker fire retardant or ferrocene.
10. the preparation method of a kind of flame-retardant wood-plastic composite material based on walnut shell flour according to claim 1 is characterized in that step is as follows,
(1) nut-shell is pulverized, made fineness reach the 40-120 order, then dry, make water content less than 2.5%, and walnut shell flour is carried out surface chemical modification process;
(2) in high-speed mixer, nano montmorillonite is joined in the walnut shell flour after step (1) surface-modifying agent is processed, processed 10-40 minute with 600-900 rpm of high-speed stirring, make the walnut shell flour of nano montmorillonite parcel;
(3) in the high-speed kneading machine, mix than the walnut shell flour with thermoplastic macromolecule resin, macromolecule modifier, thermo-stabilizer, lubricant, softening agent, composite flame-retardant agent and nano montmorillonite parcel by formulation weight, discharging after being 80-90 ℃ to temperature, then in two roller mills in 170-180 ℃ of lower melt blending 20-40 minute;
(4) the gained molten sheet drops into extrusion moulding in the screw extrusion press through cooling off fragmentation.
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| CN103214867A (en) * | 2013-04-25 | 2013-07-24 | 楚雄中信塑木新型材料有限公司 | Plastic wood taking recycled plastics and walnut shells as base materials, and processing method of plastic wood |
| CN103613823A (en) * | 2013-11-01 | 2014-03-05 | 安徽环嘉天一再生资源有限公司 | Corrosion resistant wood and plastic composite material |
| CN103740005A (en) * | 2014-01-16 | 2014-04-23 | 黑生贤 | Production formula and process of waste PVC (polyvinyl chloride) wood-plastic composition |
| CN104059371A (en) * | 2013-03-23 | 2014-09-24 | 合肥安诺新型建材有限公司 | Thermoplastic resin wood-plastic composite artificial board |
| CN104261755A (en) * | 2014-08-29 | 2015-01-07 | 明光市第二建筑安装有限责任公司 | Antibacterial environment-friendly wall thermal insulation material and preparation method thereof |
| CN104817852A (en) * | 2015-05-22 | 2015-08-05 | 罗满清 | High-strength corrosion-resistant wood-plastic composite material for plates and preparation method thereof |
| CN105062110A (en) * | 2015-07-31 | 2015-11-18 | 桂林理工大学 | Method for preparation of polypropylene based wood plastic composite material from walnut shell powder |
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| CN106046620A (en) * | 2016-07-28 | 2016-10-26 | 安吉威龙塑木环保材料有限公司 | Polyvinyl chloride plastic wood and preparation method for same |
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| CN103214867A (en) * | 2013-04-25 | 2013-07-24 | 楚雄中信塑木新型材料有限公司 | Plastic wood taking recycled plastics and walnut shells as base materials, and processing method of plastic wood |
| CN103613823A (en) * | 2013-11-01 | 2014-03-05 | 安徽环嘉天一再生资源有限公司 | Corrosion resistant wood and plastic composite material |
| CN103740005A (en) * | 2014-01-16 | 2014-04-23 | 黑生贤 | Production formula and process of waste PVC (polyvinyl chloride) wood-plastic composition |
| CN104261755A (en) * | 2014-08-29 | 2015-01-07 | 明光市第二建筑安装有限责任公司 | Antibacterial environment-friendly wall thermal insulation material and preparation method thereof |
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Application publication date: 20130102 |