CN107033458A - A kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material and preparation method thereof - Google Patents

A kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material and preparation method thereof Download PDF

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CN107033458A
CN107033458A CN201710321556.4A CN201710321556A CN107033458A CN 107033458 A CN107033458 A CN 107033458A CN 201710321556 A CN201710321556 A CN 201710321556A CN 107033458 A CN107033458 A CN 107033458A
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wood
plastic composite
polypropylene
flour
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姜洪丽
董建
卫振华
孙立平
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Taishan Medical University
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    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/005Methods for mixing in batches
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/02Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
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    • C08F255/00Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
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Abstract

The invention belongs to technical field of composite preparation, a kind of nano-graphene and APP synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material and preparation method thereof are disclosed.The problem of solving low existing wood powder/polypropylene wood-plastic composite material poor compatibility, mechanical property using APP as fire retardant, poor fire, poor heat resistance.Wood plastic composite is made up of modified wood powder, polypropylene, MA g PP, nano-graphene, APP, lubricant and other auxiliary agents.Preparation method:First, raw material is weighed;2nd, raw material mixed processing obtains premix;3rd, premix carries out melting mixing and wood plastic composite melt is made;4th, melt is by molding or hot-forming produces synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material.The present invention considerably reduces the consumption of APP, and improves the fire resistance, physical and mechanical properties and heat resistance of wood plastic composite;Technique is simple.

Description

A kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material and preparation method thereof
Technical field
The invention belongs to technical field of composite preparation, more particularly to a kind of synergistic flame-retardant wood-flour/polypropylene wood-plastic are multiple Condensation material and preparation method thereof.
Background technology
Wood plastic composite is a kind of most potential new general composite, and it is by a kind of a large amount of reproducible And cheap wood powder or wood-fibred and fluoropolymer resin are composited.Its exploitation is to protecting forest resources and ecological ring Border, makes full use of recovery waste or used plastics, and eliminating white pollution has significant economic and social benefit.But its defect is in The characteristics of wood powder and thermoplastic all have inflammable, therefore the two compound wood plastic composite prepared falls within easy fuel wood Material, directly applies to interior and there is certain potential safety hazard, which greatly limits its application field.
Although halogenated flame retardant flame retardant effect preferably, due to its it is fire-retardant during discharge poisonous and corrosive fume, Harm to environment and the mankind can not be ignored, thus development Non-halogen Flame Retardant Technology turns into one of focus of fire-retardant research field. In low cigarette, the phosphorus flame retardant of Halogen, APP (being abbreviated as APP) is because its is phosphorous, nitrogen content is high, and phosphorus-nitrogen can play collaboration Fire retarding effect, flame retardant effect is superior, and toxicity is low, using safety and overcomes that halogen containing flame-retardant smog itself is big, release gas Poisonous and many molten drops of burning the defect of body and be used widely.It is highly polar polymer, the easy moisture absorption, in wood yet with APP Dispersiveness and associativity in plastic composite materials is bad, so adding after APP, the mechanical properties decrease of composite is obvious;Separately On the one hand, APP carries out fire-retardant, addition height to wood plastic composite, and poor fire also has certain to wood plastic composite processing Influence.
Nano-graphene is a kind of New Two Dimensional nano material, has high flame retarding efficiency, environmental protection as fire retardant, does not reduce The advantages of mechanical property.Nano-graphene is added in APP, the consumption of APP, and nano-graphite can be substantially reduced Alkene and APP have cooperative effect, and both are with can improve the fire resistance of material to a greater extent, and make material Mechanical property and heat resistance are improved.
To sum up, the problem of prior art is present be:Using APP as the wood powder/polypropylene wood-plastic composite material of fire retardant Poor compatibility, low mechanical property, poor fire, poor heat resistance etc..
The content of the invention
The problem of existing for prior art, the invention provides a kind of synergistic flame-retardant wood-flour/polypropylene wood-plastic composite wood Material and preparation method thereof.
The present invention is achieved in that a kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material, the fire-retardant wood of synergistic Plastic composite materials are according to parts by weight by 30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, -6 parts of MA-g-PP3 parts, nanometer 2 parts -6 parts of graphene, 8 parts -12 parts of APP, 1 part of -2 parts of composition of 1 part -2 parts of lubricant and other auxiliary agents.
Further, the modified wood powder by 0.5 part of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide - 2 parts are made;
The MA-g-PP is by 50 parts -100 parts of polypropylene chain rupture, 20 parts -40 parts of maleic anhydride, cumyl peroxide 0.5 - 3 parts of part, 0.1 part -1 part of resistance crosslinking agent are through fusion-grafting, and extrusion, pelletizing is made;
The nano-graphene is to be made by natural flake graphite through ultrasound, washing, dry, high temperature reduction;
The lubricant includes at least one in Tissuemat E, barium stearate, zinc stearate, ethylene bis stearic acid amide Kind;
Other auxiliary agents include antioxidant, plasticizer;Wherein antioxidant is by four [β-(3,5- di-t-butyl -4- hydroxy benzenes Base) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is dioctyl phthalate or phthalic acid two Butyl ester.
Another object of the present invention is to provide a kind of preparation of the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material Method, the preparation method of the Synergetic flame-retardant wood-plastic composite material comprises the following steps:
Step one, 30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, MA-g-PP3 parts -6 are weighed according to parts by weight 1 part -2 parts of part, 8 parts -12 parts of 2 parts -6 parts of nano-graphene, APP part, 1 part -2 parts of lubricant and other auxiliary agents;Wherein, Modified wood powder is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;
Step 2, the raw material that step one is weighed is placed in stirring temperature controlling machine, stirred under the conditions of 120 DEG C -140 DEG C of temperature 2min-4min, is 3% to each material water ratio, cools the temperature to 40 DEG C -50 DEG C, obtain premix;
Step 3, the premix of step 2 is inputted in feeder, and torque rheometer is added with 5r/min feeding rotating speed, The melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature, obtains wood plastic composite melt;
Step 4, wood plastic composite melt is cooled to room temperature by molding or hot-forming, stands, that is, obtains synergistic Flame-retardant wood-flour/Polypropylene wood-plastic composite material.
Further, the preparation method of modified wood powder is in the step one:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene 0.5 part -2 parts are well mixed with di-t-butyl peroxide, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, magneton Rotating speed 60r/min-100r/min, reaction time 46h-48h.
Further, each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in the step 3, and rotor speed is 60r/min。
Further, hot pressing or wood plastic composite melt is placed in the step 4 on vulcanizing press during compression molding Sheet material is hot pressed into, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
Another object of the present invention is to provide one kind to utilize the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material system The door and window made.
Another object of the present invention is to provide one kind to utilize the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material system The floor made.
Another object of the present invention is to provide one kind to utilize the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material system The furniture material made.
Another object of the present invention is to provide one kind to utilize the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material system The automotive material made.
Compared with prior art, the present invention has following remarkable advantage:
1. the present invention is with nano-graphene and APP synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material, in poly- phosphorus Under the sour smaller addition of ammonium, the cooperative effect of nano-graphene and APP, you can increase substantially wood plastic composite Fire resistance, physical and mechanical properties and heat resistance, make the new material be better than existing flame-retardant wood in terms of properties Powder/PP composite material.
2. the present invention is using the homemade MA-g-PP in laboratory as compatilizer, chain rupture PP molecular weight is moderate, and melt fluidity is good, Before can be prior to plastic substrate wetting APP, compatilizer fully soaks APP and nano-graphene, both liftings Dispersibility and binding ability in the composite, so as to improve the mechanical property of composite.
3. the composite material and preparation method thereof of the present invention, stirring thermostat, feeder and torque rheometer cavity are combined into The equipment of complete set, it is ensured that the continuity in process, it is to avoid the loss of pilot process raw material.
4. the present invention with nano-graphene and APP synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material, its oxygen Index 27.2-32.8, is ignited time 23.9-26.6s, HRR 128-166kWm-2, impact strength 11.2- 13.3KJ·m-2, 336.6 DEG C and 518.3 DEG C of material thermal decomposition peak-peak temperature;And it is existing using APP as fire retardant Wood powder/PP composite material (40 parts of modified wood powder, 60 parts of polypropylene, MA-g-PP6 parts, APP 25 by weight Part) oxygen index (OI) be 26.2, be ignited time 22.9s, HRR 172kWm-2, impact strength 7.6KJm-2, material 326.6 DEG C and 512.3 DEG C of material thermal decomposition peak-peak temperature
To sum up, it is of the invention to have with nano-graphene and APP synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material Have the advantages that fire resistance is good, mechanical performance is high, heat-resisting good;The preparation method technique of the present invention is simple simultaneously.
Brief description of the drawings
Fig. 1 is the preparation method flow of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material provided in an embodiment of the present invention Figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
Synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material provided in an embodiment of the present invention is according to parts by weight by innovation wood 30 parts -60 parts of powder, 40 parts -70 parts of polypropylene, -6 parts of MA-g-PP3 parts, 2 parts -6 parts of nano-graphene, 8 part -12 of APP 1 part -2 parts of part, 1 part -2 parts of lubricant and other auxiliary agents;Wherein, modified wood powder by 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and 0.5 part -2 parts of di-t-butyl peroxide is made;
The MA-g-PP is by 50 parts -100 parts of polypropylene chain rupture, 20 parts -40 parts of maleic anhydride, cumyl peroxide 0.5 - 3 parts of part, 0.1 part -1 part of resistance crosslinking agent are through fusion-grafting, and extrusion, pelletizing is made;
The nano-graphene is to be made by natural flake graphite through ultrasound, washing, dry, high temperature reduction;
The lubricant includes at least one in Tissuemat E, barium stearate, zinc stearate, ethylene bis stearic acid amide Kind;
Other auxiliary agents include antioxidant, plasticizer;Wherein antioxidant is by four [β-(3,5- di-t-butyl -4- hydroxy benzenes Base) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is dioctyl phthalate or phthalic acid two Butyl ester.
As shown in figure 1, the preparation method of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material provided in an embodiment of the present invention Comprise the following steps:
S101:30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, MA-g-PP3 parts -6 are weighed according to parts by weight 1 part -2 parts of part, 8 parts -12 parts of 2 parts -6 parts of nano-graphene, APP part, 1 part -2 parts of lubricant and other auxiliary agents;Wherein, Modified wood powder is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;
S102:The step S101 raw materials weighed are placed in stirring temperature controlling machine, stirred under the conditions of 120 DEG C -140 DEG C of temperature 2min-4min, is 3% to each material water ratio, cools the temperature to 40 DEG C -50 DEG C, obtain premix;
S103:By in step S102 premix input feeder, torque rheometer is added with 5r/min feeding rotating speed, The melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature, obtains wood plastic composite melt;
S104:Wood plastic composite melt is cooled to room temperature by molding or hot-forming, stands, that is, obtains synergistic resistance Fire wood powder/polypropylene wood-plastic composite material.
The preparation method of modified wood powder is in step S101:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and peroxidating two 0.5 part -2 parts of the tert-butyl group is well mixed, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, magneton rotating speed 60r/ Min-100r/min, reaction time 46h-48h.
Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in step S103, and rotor speed is 60r/min.
Hot pressing or wood plastic composite melt is placed on vulcanizing press during compression molding in step S104 and is hot pressed into plate Material, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1
Synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material provided in an embodiment of the present invention, including following parts by weight Raw material:30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, -6 parts of MA-g-PP3 parts, 2 parts -6 parts of nano-graphene, poly- phosphorus 1 part -2 parts of sour 8 parts -12 parts of ammonium, 1 part -2 parts of lubricant and other auxiliary agents.
Embodiment 2
Lubricant is Tissuemat E, barium stearate, zinc stearate, ethylene to the embodiment of the present invention as different from Example 1 One or more combination in double stearic amides.It is other same as Example 1.
When lubricant is mixture in the embodiment of the present invention, it can be mixed by any ratio between various lubricants.
Embodiment 3
Other auxiliary agents are antioxidant, plasticizer to the embodiment of the present invention as different from Example 1;Wherein antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid] pentaerythritol ester or the double lauryls of thio-2 acid;Plasticizer is adjacent benzene Diformazan dioctyl phthalate or dibutyl phthalate.It is other same as Example 1.
Embodiment 4
The embodiment of the present invention as different from Example 3 modified wood powder by 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and mistake 0.5 part -2 parts of di-t-butyl of oxidation is made;It is other same as Example 3.
Embodiment 5
Synergistic of embodiment of the present invention flame-retardant wood-flour/Polypropylene wood-plastic composite material preparation method, synergistic flame-retardant wood-plastic is combined Material follows the steps below preparation:According to parts by weight weigh 30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, - 6 parts of MA-g-PP3 parts, 2 parts -6 parts of nano-graphene, 8 parts -12 parts of APP part, 1 part -2 parts of lubricant and other auxiliary agents 1 - 2 parts of part;Wherein, modified wood powder is by 4 parts -8 parts of wood powder, 0.5 part of -2 parts of system of 8 parts -16 parts of styrene and di-t-butyl peroxide Into;2nd, the raw material that step one is weighed is placed in stirring temperature controlling machine, 2min-4min is stirred under the conditions of 120 DEG C -140 DEG C of temperature, It is 3% to each material water ratio, cools the temperature to 40 DEG C -50 DEG C, obtain premix;3rd, the premix of step 2 is inputted into feeding In device, torque rheometer is added with 5r/min feeding rotating speed, the melting mixing 15min- under the conditions of 165 DEG C -190 DEG C of temperature 20min, obtains wood plastic composite melt;4th, wood plastic composite melt is cooled to room temperature by molding or hot-forming, Stand, that is, obtain synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material.
Lubricant in the embodiment of the present invention in step one is Tissuemat E, barium stearate, zinc stearate, ethylene are double stearic One or more combination in sour acid amides.When lubricant is mixture, it can be mixed by any ratio between various lubricants.
Other auxiliary agents are antioxidant, plasticizer in step one in the embodiment of the present invention;Wherein antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is phthalic acid two Monooctyl ester or dibutyl phthalate.
Embodiment 6
The preparation method of modified wood powder is the embodiment of the present invention in step one as different from Example 5:By 4 part -8 of wood powder - 2 parts of part, 8 parts -16 parts of styrene and hydrogen peroxidase 10 .5 parts are well mixed, nitrogen protection, and concussion reaction is to be changed at room temperature Property wood powder, rotor speed 60r/min-100r/min, reaction time 46-48 hour.Other steps and parameter and the phase of embodiment 5 Together.
Embodiment 7
The embodiment of the present invention and each area's temperature of torque rheometer in step 3 unlike embodiment 5,6 are 180 DEG C, 190 DEG C, 190 DEG C, rotor speed is 60r/min.
Embodiment 8
By wood plastic composite when the embodiment of the present invention is from hot pressing in step 4 unlike embodiment 5,6 or compression molding Melt, which is placed on vulcanizing press, is hot pressed into sheet material, and the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
Embodiment 9
Synergistic of embodiment of the present invention flame-retardant wood-flour/Polypropylene wood-plastic composite material preparation method, synergistic flame-retardant wood-plastic is combined Material follows the steps below preparation:First, 40 parts of modified wood powder, 60 parts of polypropylene, MA-g-PP6 are weighed according to parts by weight Part, 2 parts of nano-graphene, 10 parts of APP, 1 part of lubricant, other 1 part of auxiliary agents;Wherein, modified wood powder is by 4 parts of -8 parts of wood Powder, 8 parts of -16 parts of styrene and 0.5 part of -2 parts of di-t-butyl peroxide are made;2nd, the raw material that step one is weighed is placed in stirring In temperature controlling machine, 2min-4min is stirred under the conditions of 120 DEG C -140 DEG C of temperature, is 3% to each material water ratio, cools the temperature to 40 DEG C -50 DEG C, obtain premix;3rd, the premix of step 2 is inputted in feeder, torque flow is added with 5r/min feeding rotating speed Become instrument, the melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature obtains wood plastic composite melt;4th, wood moulding Composite Melt is cooled to room temperature by molding or hot-forming, stands, that is, obtains synergistic flame-retardant wood-flour/polypropylene wood-plastic Composite.
Lubricant in the embodiment of the present invention in step one is Tissuemat E, barium stearate, zinc stearate, ethylene are double stearic One or more combination in sour acid amides.When lubricant is mixture, it can be mixed by any ratio between various lubricants.
Other auxiliary agents are antioxidant, plasticizer in step one in the embodiment of the present invention;Wherein antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is phthalic acid two Monooctyl ester or dibutyl phthalate.
The preparation method of modified wood powder is in step one of the embodiment of the present invention:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene 0.5 part -2 parts are well mixed with di-t-butyl peroxide, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, rotor Rotating speed 60r/min-100r/min, reaction time 46-48 hour.
Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in step 3 of the embodiment of the present invention, and rotor speed is 60r/min。
Hot pressing or wood plastic composite melt is placed in vulcanizing press during compression molding in step 4 of the embodiment of the present invention On be hot pressed into sheet material, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
The composite property parameter that production of the embodiment of the present invention is obtained is shown in Table one.
Embodiment 10
Synergistic of embodiment of the present invention flame-retardant wood-flour/Polypropylene wood-plastic composite material preparation method, synergistic flame-retardant wood-plastic is combined Material follows the steps below preparation:First, 40 parts of modified wood powder, 60 parts of polypropylene, MA-g-PP6 are weighed according to parts by weight Part, 4 parts of nano-graphene, 10 parts of APP, 1 part of lubricant, other 1 part of part of auxiliary agent;Wherein, wherein modified wood powder is by wood powder 0.5 part -2 parts of 4 parts -8 parts, 8 parts -16 parts of styrene and di-t-butyl peroxide are made;2nd, the raw material that step one is weighed is placed in Stir in temperature controlling machine, 2min-4min is stirred under the conditions of 120 DEG C -140 DEG C of temperature, be 3% to each material water ratio, temperature is dropped To 40 DEG C -50 DEG C, premix is obtained;3rd, the premix of step 2 is inputted in feeder, is added and turned with 5r/min feeding rotating speed Square rheometer, the melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature, obtains wood plastic composite melt;4th, Wood plastic composite melt is cooled to room temperature by molding or hot-forming, stands, that is, obtains synergistic flame-retardant wood-flour/polypropylene Wood plastic composite.
Lubricant in the embodiment of the present invention in step one is Tissuemat E, barium stearate, zinc stearate, ethylene are double stearic One or more combination in sour acid amides.When lubricant is mixture, it can be mixed by any ratio between various lubricants.
Other auxiliary agents are antioxidant, plasticizer in step one in the embodiment of the present invention;Wherein antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is phthalic acid two Monooctyl ester or dibutyl phthalate.
The preparation method of modified wood powder is in step one of the embodiment of the present invention:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene 0.5 part -2 parts are well mixed with di-t-butyl peroxide, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, rotor Rotating speed 60r/min-100r/min, reaction time 46-48 hour.
Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in step 3 of the embodiment of the present invention, and rotor speed is 60r/min。
Hot pressing or wood plastic composite melt is placed in vulcanizing press during compression molding in step 4 of the embodiment of the present invention On be hot pressed into sheet material, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
The composite property parameter that production of the embodiment of the present invention is obtained is shown in Table one.
Embodiment 11
Synergistic of embodiment of the present invention flame-retardant wood-flour/Polypropylene wood-plastic composite material preparation method, synergistic flame-retardant wood-plastic is combined Material follows the steps below preparation:First, 30 parts of modified wood powder, 70 parts of polypropylene, MA-g-PP6 are weighed according to parts by weight Part, 4 parts of nano-graphene, 10 parts of APP, 1 part -2 parts of lubricant, other 1 part -2 parts of auxiliary agents;Wherein, wherein modified wood powder It is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;2nd, the original for weighing step one Material is placed in stirring temperature controlling machine, and 2min-4min is stirred under the conditions of 120 DEG C -140 DEG C of temperature, is 3% to each material water ratio, will Temperature is down to 40 DEG C -50 DEG C, obtains premix;3rd, the premix of step 2 is inputted in feeder, with 5r/min feeding rotating speed Torque rheometer is added, the melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature obtains wood plastic composite and melted Body;4th, wood plastic composite melt by molding or it is hot-forming, be cooled to room temperature, stand, that is, obtain synergistic flame-retardant wood-flour/ Polypropylene wood-plastic composite material.
Lubricant in the embodiment of the present invention in step one is Tissuemat E, barium stearate, zinc stearate, ethylene are double stearic One or more combination in sour acid amides.When lubricant is mixture, it can be mixed by any ratio between various lubricants.
Other auxiliary agents are antioxidant, plasticizer in step one in the embodiment of the present invention;Wherein antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is phthalic acid two Monooctyl ester or dibutyl phthalate.
The preparation method of modified wood powder is in step one of the embodiment of the present invention:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene 0.5 part -2 parts are well mixed with di-t-butyl peroxide, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, rotor Rotating speed 60r/min-100r/min, reaction time 46-48 hour.
Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in step 3 of the embodiment of the present invention, and rotor speed is 60r/min。
Hot pressing or wood plastic composite melt is placed in vulcanizing press during compression molding in step 4 of the embodiment of the present invention On be hot pressed into sheet material, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
The composite property parameter that production of the embodiment of the present invention is obtained is shown in Table one.
Embodiment 12
Synergistic of embodiment of the present invention flame-retardant wood-flour/Polypropylene wood-plastic composite material preparation method, synergistic flame-retardant wood-plastic is combined Material follows the steps below preparation:First, 40 parts of modified wood powder, 60 parts of polypropylene, MA-g-PP6 are weighed according to parts by weight Part, 4 parts of nano-graphene, 10 parts of APP, 1 part -2 parts of lubricant, other 1 part -2 parts of auxiliary agents;Wherein, wherein modified wood powder It is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;2nd, the original for weighing step one Material is placed in stirring temperature controlling machine, and 2min-4min is stirred under the conditions of 120 DEG C -140 DEG C of temperature, is 3% to each material water ratio, will Temperature is down to 40 DEG C -50 DEG C, obtains premix;3rd, the premix of step 2 is inputted in feeder, with 5r/min feeding rotating speed Torque rheometer is added, the melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of temperature obtains wood plastic composite and melted Body;4th, wood plastic composite melt by molding or it is hot-forming, be cooled to room temperature, stand, that is, obtain synergistic flame-retardant wood-flour/ Polypropylene wood-plastic composite material.
Lubricant in the embodiment of the present invention in step one is Tissuemat E, barium stearate, zinc stearate, ethylene are double stearic One or more combination in sour acid amides.When lubricant is mixture, it can be mixed by any ratio between various lubricants.
Other auxiliary agents are antioxidant, plasticizer in step one in the embodiment of the present invention;Wherein antioxidant is four [β-(3,5- Di-tert-butyl-hydroxy phenyl) propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is phthalic acid two Monooctyl ester or dibutyl phthalate.
The preparation method of modified wood powder is in step one of the embodiment of the present invention:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene 0.5 part -2 parts are well mixed with di-t-butyl peroxide, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, rotor Rotating speed 60r/min-100r/min, reaction time 46-48 hour.
Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in step 3 of the embodiment of the present invention, and rotor speed is 60r/min。
Hot pressing or wood plastic composite melt is placed in vulcanizing press during compression molding in step 4 of the embodiment of the present invention On be hot pressed into sheet material, the temperature of upper lower platen is 165 DEG C, 10 minutes press times.
The composite property parameter that production of the embodiment of the present invention is obtained is shown in Table one.
Performance test
Performance test is carried out to synergistic flame-retardant wood-flour/PP composite material obtained by embodiments of the invention 9-12, as a result It is shown in Table one.
The synergistic flame-retardant wood-flour of table one/Properties of Polypropylene Composite test data
Test event Embodiment 9 Embodiment 10 Embodiment 11 Embodiment 12
Oxygen index (OI)/% 27.2 28.6 29.7 32.8
Burning time/s 23.9 24.2 23.7 26.6
Peak value HRR/kWm-2 166 163 158 128
Impact strength/KJm-2 11.8 12.6 13.2 11.2
The performance data test specification of table one:Oxygen index (OI) is tested by ASTM D 2836 standard method;Burning time, Peak value HRR is tested according to ISO5600-1-2002 standard;Impact strength is tested according to GB/T1843-1996.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.

Claims (10)

1. a kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material, it is characterised in that the synergistic flame-retardant wood-flour/polypropylene Wood plastic composite according to parts by weight by 30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, -6 parts of MA-g-PP3 parts, receive 2 parts -6 parts of graphene of rice, 8 parts -12 parts of APP part, 1 part of -2 parts of composition of 1 part -2 parts of lubricant and other auxiliary agents.
2. synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material as claimed in claim 1, it is characterised in that the innovation wood Powder is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;
The MA-g-PP is by 50 parts -100 parts of polypropylene chain rupture, 20 parts -40 parts of maleic anhydride, 0.5 part -3 of cumyl peroxide Part, 0.1 part -1 part of resistance crosslinking agent are through fusion-grafting, and extrusion, pelletizing is made;
The nano-graphene is to be made by natural flake graphite through ultrasound, washing, dry, high temperature reduction;
The lubricant includes at least one of Tissuemat E, barium stearate, zinc stearate, ethylene bis stearic acid amide;
Other auxiliary agents include antioxidant, plasticizer;Wherein antioxidant is by four [β-(3,5- di-tert-butyl-hydroxy phenyls) Propionic acid] the double lauryls of pentaerythritol ester or thio-2 acid;Plasticizer is dioctyl phthalate or the fourth of phthalic acid two Ester.
3. a kind of preparation method of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material as claimed in claim 1, its feature exists In the preparation method of the synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material comprises the following steps:
Step one, according to parts by weight weigh 30 parts -60 parts of modified wood powder, 40 parts -70 parts of polypropylene, -6 parts of MA-g-PP3 parts, 1 part -2 parts of 2 parts -6 parts of nano-graphene, 8 parts -12 parts of APP, 1 part -2 parts of lubricant and other auxiliary agents;Wherein, innovation wood Powder is made up of 0.5 part -2 parts of 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide;
Step 2, the raw material that step one is weighed is placed in stirring temperature controlling machine, 2min- is stirred under the conditions of 120 DEG C -140 DEG C of temperature 4min, is 3% to each material water ratio, cools the temperature to 40 DEG C -50 DEG C, obtain premix;
Step 3, the premix of step 2 is inputted in feeder, and torque rheometer, Yu Wen are added with 5r/min feeding rotating speed Melting mixing 15min-20min under the conditions of 165 DEG C -190 DEG C of degree, obtains wood plastic composite melt;
Step 4, wood plastic composite melt is cooled to room temperature by molding or hot-forming, stands, that is, obtains synergistic fire-retardant Wood powder/polypropylene wood-plastic composite material.
4. the preparation method of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material as claimed in claim 3, it is characterised in that institute The preparation method for stating modified wood powder in step one is:By 4 parts -8 parts of wood powder, 8 parts -16 parts of styrene and di-t-butyl peroxide 0.5 part -2 parts are well mixed, nitrogen protection, and concussion reaction is to obtain modified wood powder at room temperature, magneton rotating speed 60r/min-100r/ Min, reaction time 46h-48h.
5. the preparation method of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material as claimed in claim 3, it is characterised in that Each area's temperature of torque rheometer is 180 DEG C, 190 DEG C, 190 DEG C in the step 3, and rotor speed is 60r/min.
6. described in hot pressing or wood plastic composite melt is placed on vulcanizing press during compression molding and is hot pressed into plate in step 4 Material, the temperature of upper lower platen is 160 DEG C, 10 minutes press times.
7. a kind of door of synergistic flame-retardant wood-flour described in utilization claim 1~2 any one/Polypropylene wood-plastic composite material manufacture Window.
8. a kind of ground of synergistic flame-retardant wood-flour described in utilization claim 1~2 any one/Polypropylene wood-plastic composite material manufacture Plate.
9. a kind of family of synergistic flame-retardant wood-flour described in utilization claim 1~2 any one/Polypropylene wood-plastic composite material manufacture Has material.
10. a kind of synergistic flame-retardant wood-flour described in utilization claim 1~2 any one/Polypropylene wood-plastic composite material manufacture Automotive material.
CN201710321556.4A 2017-05-09 2017-05-09 A kind of synergistic flame-retardant wood-flour/Polypropylene wood-plastic composite material and preparation method thereof Pending CN107033458A (en)

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