CN102093735A - Wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as fire retardant and preparation method thereof - Google Patents
Wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as fire retardant and preparation method thereof Download PDFInfo
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- CN102093735A CN102093735A CN2011100217378A CN201110021737A CN102093735A CN 102093735 A CN102093735 A CN 102093735A CN 2011100217378 A CN2011100217378 A CN 2011100217378A CN 201110021737 A CN201110021737 A CN 201110021737A CN 102093735 A CN102093735 A CN 102093735A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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Abstract
The invention relates to a wood flour/polypropylene wood-plastic composite material and a preparation method thereof, in particular to a wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as a fire retardant and a preparation method thereof. The invention solves the problems of poor compatibility, low mechanical properties, poor fire retardance and poor heat resistance of the existing wood flour/polypropylene wood-plastic composite material using ammonium polyphosphate as a fire retardant. The wood-plastic composite material is prepared from wood flour, polypropylene, silane modified ammonium polyphosphate, m-TMI-g-PP coupling agent and antioxidant, wherein the silane modified ammonium polyphosphate is prepared from ammonium polyphosphate and gamma-methacryloxypropyltrimethoxysilane. The preparation method comprises the following steps: preparing the silane modified ammonium polyphosphate; then, mixing the wood flour, polypropylene, silane modified ammonium polyphosphate, m-TMI-g-PP coupling agent and antioxidant; and finally, extruding by using a double screw extruder. The wood-plastic composite material provided by the invention has fine fire retardance, high mechanical properties and good heat resistance; and the process is simple.
Description
Technical field
The present invention relates to a kind of wood powder/polypropylene wood plastic composite materials and preparation method thereof, being specifically related to silane-modified ammonium polyphosphate is wood powder/polypropylene wood plastic composite materials of fire retardant and preparation method thereof.
Background technology
Wood plastic composite is to utilize the agricultural waste wood raw material and the plastics of different constituent element forms or reclaim a kind of environmentally friendly novel material of plastics by technique means formation such as recombinating, compound.The wood plastic composite development is very fast after the nineties in last century, and it is mainly used in exterior finish, claustra plate, stair, guardrail and a small amount of civilian consumer's goods.The waste plastic raw material that wood plastic composite can make full use of waste and old wood material and be difficult to degrade provides new solution route for alleviating present timber resources problem deficient and the technics of reclaim of plastic waste utilization.Must consider that lignocellulosic material quickens the pyrolytic characteristic more than 200 ℃ during plastic raw materials that wood plastic composite is selected, the plastic material fusing point can not be too high.The most frequently used plastics variety comprises high density polyethylene(HDPE) (HDPE), polypropylene (PP), polystyrene (PS) and polyvinyl chloride (PVC) at present.Except that PVC, lignocellulosic material and other three kinds of plastics all belong to inflammable material, can not reach the code for fire prevention design of interior decoration of buildings requirement without fire-retardant finish, are used for the certain disaster hidden-trouble of indoor existence.Wood plastic composite is studied its combustioncharacteristics as a kind of emerging and widely used material, and rationally carrying out fire-retardant finish is its use range of expansion, makes one of important means of product diversification.
Though traditional halogenated flame retardant flame retardant effect is better, owing to discharge poisonous and corrosive hydrogen halide in its fire-retardant process, environment and human harm be can not be ignored, thereby the development Non-halogen Flame Retardant Technology becomes one of focus of fire-retardant research field.Especially the most noticeable with the applied research of ammonium polyphosphate (being called for short APP) in the phosphorus flame retardant of low cigarette, halogen.Phosphorous because of it, nitrogen content is high, phosphorus-nitrogen can be brought into play the cooperative flame retardant effect, flame retardant effect is superior, toxicity is low simultaneously, safe in utilization, overcome the defective that the smog of halogen containing flame-retardant own is big, emit deleterious corrosive gases and many molten drops that burn, but studies show that because APP is high polar polymkeric substance, dispersiveness and associativity in wood plastic composite are bad, so the mechanical properties decrease of matrix material behind the adding APP, the tensile strength of matrix material, flexural strength and shock strength all obviously descend.It is fire-retardant to studies show that simultaneously APP carries out wood plastic composite, poor effect, and the addition height has certain influence to wood plastic composite processing and mechanical property etc.
Summary of the invention
The objective of the invention is in order to solve existing is that the consistency of wood powder/polypropylene wood plastic composite materials of fire retardant is poor, mechanical property is low, flame retardant properties is poor, the problem of resistance toheat difference with the ammonium polyphosphate, the invention provides a kind of is the wood powder/polypropylene wood plastic composite materials and preparation method thereof of fire retardant with silane-modified ammonium polyphosphate, has obtained having simultaneously the wood plastic composite of good consistency, mechanical property, resistance toheat and flame retardant properties.
Of the present invention is the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, by weight by 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of silane-modified ammonium polyphosphates (M-APP), 3～6 parts of m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 0.1～1 part of oxidation inhibitor are made, and described silane-modified ammonium polyphosphate is to be made by 80～100 parts of ammonium polyphosphates and 0.5～2 part of γ-methacryloxypropyl trimethoxy silane by weight.
Of the present invention is that the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant realizes by following steps with silane-modified ammonium polyphosphate: one, by weight 80～100 parts of ammonium polyphosphates, 0.5～2 part of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol are put into there-necked flask, stir 1h down at 60 ℃, suction filtration then, then filter cake is placed baking oven, under 105 ℃ of conditions, dry 3h, get silane-modified ammonium polyphosphate (M-APP), wherein the ratio of ammonium polyphosphate weight and dehydrated alcohol volume is 80～100g: 150mL; Two, take by weighing following raw material by weight: silane-modified ammonium polyphosphate, 3～6 parts of m-pseudoallyl-α of 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 0.1～1 part of oxidation inhibitor; Three, the raw material mixing and stirring that step 2 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that silane-modified ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
The present invention is with silane coupling agent (γ-methacryloxypropyl trimethoxy silane, KH-570) ammonium polyphosphate modifying (abbreviating M-APP as) is a halogen-free flame retardants, improve flame retardant properties, physical and mechanical properties and the resistance toheat of wood powder/polypropylene composite material significantly, improved the consistency between silane-modified ammonium polyphosphate and the wood powder, made this novel material all be better than existing flame retardant type wood powder/polypropylene composite material at every aspect of performance.
The present invention is with the KH-570 ammonium polyphosphate modifying, and KH-570 has improved the interface compatibility and the dispersiveness of ammonium polyphosphate (APP), has improved dispersive ability and the binding ability of APP in matrix material, thereby has improved the mechanical property of matrix material.
Of the present invention is that the wood powder/polypropylene wood plastic composite materials of fire retardant is in being subjected to thermal process with silane-modified ammonium polyphosphate, silane-modified ammonium polyphosphate (M-APP) discharges phosphoric acid, HPO free radical, PO free radical, Si-O, Si-C and organic group etc., they can catch the free radical that wood powder discharges, make wood powder accelerate to resolve into charcoal, make the wood powder resolving time in advance, thereby make polypropylene become stable, postpone decomposition and reach flame retardant effect.M-APP can promote the charcoal layer to generate simultaneously; stop the heat passage and inflammable gas exchange in the combustion processes, can be stable at the high temperature protection polypropylene, its decomposition temperature is postponed; this shows, add the M-APP fire retardant thermal destruction behavior of matrix material is better improved.
Of the present invention is that the mechanical property of wood powder/polypropylene wood plastic composite materials (brief note be M-APP wood powder/PP material) of fire retardant is good with silane-modified ammonium polyphosphate, tensile strength is 24.93～28.04MPa, flexural strength is 61.98～65.68MPa, and shock strength is 4.11～5.75kJ/m
2And existing be that (brief note is APP wood powder/PP material for the wood powder/polypropylene wood plastic composite materials of fire retardant with the ammonium polyphosphate, make by 25 parts of APP, 60 parts of wood powders, 40 parts of PP, 6 parts of m-TMI-g-PP coupling agents and 1 part of oxidation inhibitor by weight) tensile strength be 21.88MPa, flexural strength is 59.87MPa, and shock strength is 3.39kJ/m
2The tensile strength that does not add the wood powder/polypropylene wood plastic composite materials (brief note is wood powder/PP material) of fire retardant is 23.27MPa, and flexural strength is 60.29MPa, and shock strength is 3.94kJ/m
2As seen, the mechanical property of M-APP wood powder of the present invention/PP material is better than the mechanical property of existing APP wood powder/PP material and wood powder/PP material, has solved existing because the adding of ammonium polyphosphate flame retardant causes the problem of the mechanical properties decrease of wood powder/PP material.
The resistance toheat of M-APP wood powder of the present invention/PP material is good, and the initial resolving time shortens, and has promoted M-APP wood powder/PP material to become charcoal.Temperature (the T during weight loss 1% of M-APP wood powder of the present invention/PP material
1wt%) be 102.3～108.3 ℃, decompose climax temperature value (T
Max1) be 322.9～339.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 499.6～519.6 ℃, the carbon residue quality in the time of 800 ℃ is 21.3%～22.7%.Being better than existing is the resistance toheat (T of the wood powder/polypropylene wood plastic composite materials (being made by 25 parts of APP, 60 parts of wood powders, 40 parts of PP, 6 parts of m-TMI-g-PP coupling agents and 1 part of oxidation inhibitor by weight) of fire retardant with the ammonium polyphosphate
1wt%Be 110.7 ℃, T
Max1Be 329.3 ℃, T
Max2The carbon residue quality is 20.5% when being 518.0 ℃ and 800 ℃) resistance toheat.
The flame retardant properties of M-APP wood powder of the present invention/PP material is good, and limiting oxygen index(LOI) is 28.3%～30.7%, and burning time (TTI) reaches 36～56s, and (HRR) is little for heat release rate, is 154.9～169.7kW/m
2, total heat burst size (THR) numerical value is little, 57.2～62.2MJ/m
2All being better than existing is that (limiting oxygen index(LOI) is 27.4%, TTI is that 28s, HRR are 196.2kW/m for the flame retardant properties of the wood powder/polypropylene wood plastic composite materials (being made by 25 parts of APP, 60 parts of wood powders, 40 parts of PP, 6 parts of m-TMI-g-PP coupling agents and 1 part of oxidation inhibitor by weight) of fire retardant with the ammonium polyphosphate
2, THR is 72MJ/m
2).
To sum up, of the present invention is that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate; Simultaneously, preparation method's technology of the present invention is simple.
Description of drawings
Fig. 1 be embodiment 14,15 and 16 be heat release rate (HRR)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, curve 1 is an embodiment 14 among the figure, curve 2 is embodiment 15, and curve 3 is an embodiment 16;
Fig. 2 is total heat burst size (THR)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of embodiment 14,15 and 16, curve 1 is an embodiment 14 among the figure, curve 2 is embodiment 15, and curve 3 is an embodiment 16;
Fig. 3 is total smoke release (TSP)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of embodiment 14,15 and 16, curve 1 is an embodiment 14 among the figure, curve 2 is embodiment 15, and curve 3 is an embodiment 16;
Fig. 4 is the thermogravimetric curve figure of the wood powder/polypropylene wood plastic composite materials of embodiment 16,17 and 18, curve 1 is an embodiment 16 among the figure, curve 2 is an embodiment 17, and curve 3 is an embodiment 18;
Fig. 5 is the difference quotient thermogravimetric curve figure of the wood powder/polypropylene wood plastic composite materials of embodiment 16,17 and 18, curve 1 is an embodiment 16 among the figure, curve 2 is an embodiment 17, and curve 3 is an embodiment 18;
Fig. 6 is heat release rate (HRR)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of embodiment 16,17 and 18, curve 1 is an embodiment 17 among the figure, curve 2 is embodiment 18, and curve 3 is an embodiment 16;
Fig. 7 is total heat burst size (THR)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of embodiment 16,17 and 18, curve 1 is an embodiment 17 among the figure, curve 2 is embodiment 18, and curve 3 is an embodiment 16;
Fig. 8 is total smoke release (TSP)-time (s) graphic representation of the wood powder/polypropylene wood plastic composite materials of embodiment 16,17 and 18, curve 1 is an embodiment 17 among the figure, curve 2 is embodiment 18, and curve 3 is an embodiment 16;
Fig. 9 be embodiment 16 be the scanning electron photomicrograph that the wood powder/polypropylene wood plastic composite materials of fire retardant carries out the surperficial charcoal layer after the flame retardant properties test with silane-modified ammonium polyphosphate;
Figure 10 be embodiment 17 be the scanning electron photomicrograph that the wood powder/polypropylene wood plastic composite materials of fire retardant carries out the surperficial charcoal layer after the flame retardant properties test with the ammonium polyphosphate.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by weight by 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of silane-modified ammonium polyphosphates (M-APP), 3～6 parts of m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 0.1～1 part of oxidation inhibitor are made, and described silane-modified ammonium polyphosphate is to be made by 80～100 parts of ammonium polyphosphates and 0.5～2 part of γ-methacryloxypropyl trimethoxy silane by weight.
Present embodiment be that the mechanical property of wood powder/polypropylene wood plastic composite materials of fire retardant is good with silane-modified ammonium polyphosphate, tensile strength is 24.93～28.04MPa, flexural strength is 61.98～65.68MPa, shock strength is 4.11～5.75kJ/m
2Resistance toheat is good, the temperature (T during weight loss 1%
1wt%) be 102.3～108.3 ℃, decompose climax temperature value (T
Max1) be 322.9～339.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 499.6～519.6 ℃, the carbon residue quality in the time of 800 ℃ is 21.3%～22.7%; Flame retardant properties is good, and limiting oxygen index(LOI) is 28.3%～30.7%, and burning time (TTI) reaches 36～56s, and (HRR) is little for heat release rate, is 154.9～169.7kW/m
2, total heat burst size (THR) numerical value is little, 57.2～62.2MJ/m
2
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.
Embodiment two: present embodiment and embodiment one are different is by weight by 60 parts of wood powders, 40 parts of polypropylene, 20 parts of silane-modified ammonium polyphosphates, 6 parts of m-pseudoallyl-α, and α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor are made.Other parameter is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is by weight by 60 parts of wood powders, 40 parts of polypropylene, 25 parts of silane-modified ammonium polyphosphates, 6 parts of m-pseudoallyl-α, and α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor are made.Other parameter is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one, two or three were different is that described silane-modified ammonium polyphosphate is to be made by 90～100 parts of ammonium polyphosphates and 1～2 part of γ-methacryloxypropyl trimethoxy silane by weight.Other parameter is identical with embodiment one, two or three.
Embodiment five: what present embodiment and embodiment one, two or three were different is that described silane-modified ammonium polyphosphate is to be made by 100 parts of ammonium polyphosphates and 1.5 parts of γ-methacryloxypropyl trimethoxy silane by weight.Other parameter is identical with embodiment one, two or three.
Embodiment six: what present embodiment was different with one of embodiment one to five is that described oxidation inhibitor is antioxidant 1010, antioxidant 1076 or oxidation inhibitor 168.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is described in the embodiment one to be the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is realized by following steps: one, by weight with 80～100 parts of ammonium polyphosphates, 0.5～2 parts of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol are put into there-necked flask, stir 1h down at 60 ℃, suction filtration then, then filter cake is placed baking oven, under 105 ℃ of conditions, dry 3h, get silane-modified ammonium polyphosphate (M-APP), wherein the ratio of ammonium polyphosphate weight and dehydrated alcohol volume is 80～100g: 150mL; Two, take by weighing following raw material by weight: silane-modified ammonium polyphosphate, 3～6 parts of m-pseudoallyl-α of 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 0.1～1 part of oxidation inhibitor; Three, the raw material mixing and stirring that step 2 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that silane-modified ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
Preparation method's technology of present embodiment is simple.What prepare is that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 24.93～28.04MPa, and flexural strength is 61.98～65.68MPa, and shock strength is 4.11～5.75kJ/m
2Resistance toheat is good, the temperature (T during weight loss 1%
1wt%) be 102.3～108.3 ℃, decompose climax temperature value (T
Max1) be 322.9～339.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 499.6～519.6 ℃, the carbon residue quality in the time of 800 ℃ is 21.3%～22.7%; Flame retardant properties is good, and limiting oxygen index(LOI) is 28.3%～30.7%, and burning time (TTI) reaches 36～56s, and (HRR) is little for heat release rate, is 154.9～169.7kW/m
2, total heat burst size (THR) numerical value is little, 57.2～62.2MJ/m
2
The standard of the weight part in the present embodiment in step 1 and the step 2 can be different.
Embodiment eight: present embodiment and embodiment seven are different is by weight 90～100 parts of ammonium polyphosphates, 1～2 part of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol to be put into there-necked flask in the step 1.Other step and parameter are identical with embodiment seven.
Embodiment nine: present embodiment and embodiment seven are different is by weight 100 parts of ammonium polyphosphates, 1.5 parts of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol to be put into there-necked flask in the step 1.Other step and parameter are identical with embodiment seven.
Embodiment ten: what present embodiment and embodiment seven, eight or nine were different is to take by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 20 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.Other step and parameter are identical with embodiment seven, eight or nine.
Embodiment 11: what present embodiment and embodiment seven, eight or nine were different is to take by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 25 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.Other step and parameter are identical with embodiment seven, eight or nine.
Embodiment 12: what present embodiment and embodiment seven, eight or nine were different is to take by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 15 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.Other step and parameter are identical with embodiment seven, eight or nine.
Embodiment 13: what present embodiment and embodiment seven, eight or nine were different is to take by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 30 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.Other step and parameter are identical with embodiment seven, eight or nine.
Embodiment 14: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 15g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 1.5g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 26.62MPa, and flexural strength is 64.25MPa, and shock strength is 4.90kJ/m
2Resistance toheat is good, the temperature (T during weight loss 1%
1wt%) be 108.3 ℃, decompose climax temperature value (T
Max1) be 339.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 499.6 ℃, the carbon residue quality in the time of 800 ℃ is 21.3%; Flame retardant properties is good, and limiting oxygen index(LOI) is 28.3%, and burning time (TTI) reaches 36s, and (HRR) is little for heat release rate, is 169.7kW/m
2, total heat burst size (THR) numerical value is little, 62.2MJ/m
2
Present embodiment be that heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 11 with silane-modified ammonium polyphosphate.
Present embodiment be that total heat burst size (THR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 21 with silane-modified ammonium polyphosphate.
Present embodiment be that total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 31 with silane-modified ammonium polyphosphate.
Present embodiment be the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, realize by following steps: one, by weight 100g ammonium polyphosphate, 1.5g γ-methacryloxypropyl trimethoxy silane and 150mL dehydrated alcohol are put into there-necked flask, stir 1h down at 60 ℃, suction filtration then, then filter cake is placed baking oven, under 105 ℃ of conditions, dry 3h, get silane-modified ammonium polyphosphate (M-APP); Two, take by weighing following raw material by weight: silane-modified ammonium polyphosphate, the 6g m-pseudoallyl-α of 60g wood powder, 40g polypropylene, the preparation of 15g step 1, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1g antioxidant 1010; Three, the raw material mixing and stirring that step 2 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that silane-modified ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
Embodiment 15: present embodiment and embodiment 14 are different be with silane-modified ammonium polyphosphate be the wood powder/polypropylene wood plastic composite materials of fire retardant by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 20g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made.Other parameter is identical with embodiment 14.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 27.1MPa, and flexural strength is 65.68MPa, and shock strength is 5.50kJ/m
2Resistance toheat is good, the temperature (T during weight loss 1%
1wt%) be 104.7 ℃, decompose climax temperature value (T
Max1) be 326.7 ℃, polypropylene decomposes climax temperature value (T
Max2) be 512.3 ℃, the carbon residue quality in the time of 800 ℃ is 22%; Flame retardant properties is good, and limiting oxygen index(LOI) is 29.5%, and burning time (TTI) reaches 54s, and (HRR) is little for heat release rate, is 158.7kW/m
2, total heat burst size (THR) numerical value is little, 58.8MJ/m
2
Present embodiment be that heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 12 with silane-modified ammonium polyphosphate.
Present embodiment be that total heat burst size (THR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 22 with silane-modified ammonium polyphosphate.
Present embodiment be that total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 32 with silane-modified ammonium polyphosphate.
Present embodiment be that the preparation method of record in preparation method and the embodiment 14 of wood powder/polypropylene wood plastic composite materials of fire retardant compares with silane-modified ammonium polyphosphate, the silane-modified ammonium polyphosphate that takes by weighing in step 2 is changed into the 20g, and remaining step and parameter are the same.
Embodiment 16: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 25g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 1.5g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the preparation method of record in preparation method and the embodiment 14 of wood powder/polypropylene wood plastic composite materials of fire retardant compares with silane-modified ammonium polyphosphate, the silane-modified ammonium polyphosphate that takes by weighing in step 2 is changed into the 25g, and remaining step and parameter are the same.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 28.04MPa, and flexural strength is 65.53MPa, and shock strength is 5.75kJ/m
2Resistance toheat is good, the temperature (T during weight loss 1%
1wt%) be 102.3 ℃, decompose climax temperature value (T
Max1) be 322.9 ℃, polypropylene decomposes climax temperature value (T
Max2) be 519.6 ℃, the carbon residue quality in the time of 800 ℃ is 22.7%; Flame retardant properties is good, and limiting oxygen index(LOI) is 30.7%, and burning time (TTI) reaches 56s, and (HRR) is little for heat release rate, is 154.9kW/m
2, total heat burst size (THR) numerical value is little, 57.2MJ/m
2
Present embodiment be that heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 13 with silane-modified ammonium polyphosphate.
In the synthesizing map 1 each curve as seen, along with the increase of M-APP consumption, heat release rate (HRR) obviously descends, by 169.7kW/m in the embodiment 14 to 16
2Drop to 154.9kW/m
2When the M-APP consumption was 20 parts, wood plastic composite showed good flame-retardant effect, continued to improve the consumption of M-APP, and the reduction amplitude of HRR diminishes.
Present embodiment be that total heat burst size (THR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 23 with silane-modified ammonium polyphosphate.
In the synthesizing map 2 each curve as seen, along with the increase of M-APP consumption, total heat burst size (THR) obviously diminishes in the embodiment 14 to 16, when the M-APP consumption was 25 parts, reducing of total heat burst size was not obvious.
Present embodiment be that total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 33 with silane-modified ammonium polyphosphate.
In the synthesizing map 3 each curve as seen, along with the increase of M-APP consumption, total smoke release (TSP) obviously reduces in the embodiment 14 to 16, when the M-APP consumption was 25 parts, reducing of total heat burst size was not obvious.
What simultaneously, adopt present embodiment that the thermogravimetric analyzer test obtains is that the thermogravimetric curve (TG curve) of wood powder/polypropylene wood plastic composite materials of fire retardant and difference quotient thermogravimetric curve (DTG curve) are respectively shown in curve 1 among curve among Fig. 41 and Fig. 5 with silane-modified ammonium polyphosphate.
Adopt the taper calorimeter, carry out according to ASTM 1356-90 standard the present embodiment after the flame retardant properties test wood plastic composite surperficial charcoal layer scanning electron photomicrograph as shown in Figure 9.As seen from Figure 9; the matrix material burning surface charcoal layer that adds M-APP is more bulk; the thicker thicker protective membrane of material surface generation that makes of charcoal layer stops spreading of the intensity of a fire; as seen KH-570 can improve the dispersed and combination row of APP in matrix material; promote that wood powder becomes charcoal; stop transfer of heat to prevent simultaneously that to polypropylene (PP) oxygen from entering material internal and making it combustion-supporting; charcoal layer structure is the primary factor of fire retardancy; again in conjunction with the data analysis of taper calorimeter; the raising of mechanical property illustrates that M-APP has improved material incessantly in wood plastic composite mechanical property has improved flame retardant properties simultaneously.
Embodiment 17: present embodiment is comparative example one: ammonium polyphosphate is the wood powder/polypropylene wood plastic composite materials of fire retardant, it is by 60g wood powder, 40g polypropylene, 25g ammonium polyphosphate (APP), 6g m-pseudoallyl-α, and α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made.
The preparation method is: one, take by weighing following raw material by weight: 60g wood powder, 40g polypropylene, 25g ammonium polyphosphate, 6gm-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1g antioxidant 1010; Two, the raw material mixing and stirring that step 1 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
Present embodiment is a fire retardant not adopt silane-modified ammonium polyphosphate, and mechanical property parameters is: tensile strength is 21.88MPa, and flexural strength is 59.87MPa, and shock strength is 3.39kJ/m
2The resistance toheat parameter is: the temperature (T during weight loss 1%
1wt%) be 110.7 ℃, decompose climax temperature value (T
Max1) be 329.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 518.0 ℃, the carbon residue quality in the time of 800 ℃ is 21.5%; The flame retardant properties parameter is: limiting oxygen index(LOI) is 27.4%, and burning time (TTI) reaches 28s, and (HRR) is little for heat release rate, is 196.2kW/m
2, total heat burst size (THR) numerical value is little, 72MJ/m
2
What adopt present embodiment that the thermogravimetric analyzer test obtains is that the thermogravimetric curve (TG curve) of wood powder/polypropylene wood plastic composite materials of fire retardant and difference quotient thermogravimetric curve (DTG curve) are respectively shown in curve 2 among curve among Fig. 42 and Fig. 5 with the ammonium polyphosphate.Curve 2 and curve 1 400 ℃ of corresponding later curves almost overlap among Fig. 5.
Present embodiment be that heat release rate (HRR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 61 with ammonium polyphosphate (APP).
Present embodiment be that total heat burst size (THR)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 71 with the ammonium polyphosphate.
Present embodiment be that total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is shown in curve among Fig. 81 with the ammonium polyphosphate.
Adopt the taper calorimeter, carry out according to ASTM 1356-90 standard the present embodiment after the flame retardant properties test wood plastic composite surperficial charcoal layer scanning electron photomicrograph as shown in figure 10.As seen from Figure 10, surperficial charcoal layer is thin and fine and close.
Embodiment 18: present embodiment is comparative example two: the wood powder/polypropylene wood plastic composite materials that does not add fire retardant, it is by 60g wood powder, 40g polypropylene, 6g m-pseudoallyl-α, and α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made.
The preparation method is: one, take by weighing following raw material by weight: 60g wood powder, 40g polypropylene, 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1g antioxidant 1010; Two, the raw material mixing and stirring that step 1 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly got wood powder/polypropylene wood plastic composite materials.
Wood powder/polypropylene wood plastic composite materials that present embodiment does not adopt fire retardant to prepare, mechanical property parameters is: tensile strength is 23.27MPa, and flexural strength is 60.29MPa, and shock strength is 3.94kJ/m
2The resistance toheat parameter is: the temperature (T during weight loss 1%
1wt%) be 118.4 ℃, decompose climax temperature value (T
Max1) be 383.2 ℃, polypropylene decomposes climax temperature value (T
Max2) be 444.8 ℃, the carbon residue quality in the time of 800 ℃ is 12.6%; The flame retardant properties parameter is: limiting oxygen index(LOI) is 23.6%, and burning time (TTI) reaches 33s, and heat release rate (HRR) is big, is 357.5kW/m
2, total heat burst size (THR) numerical value is big, 102.1MJ/m
2
The thermogravimetric curve (TG curve) of the wood powder that the does not add fire retardant/polypropylene wood plastic composite materials of the present embodiment that the test of employing thermogravimetric analyzer obtains and difference quotient thermogravimetric curve (DTG curve) are respectively shown in curve 3 among curve among Fig. 43 and Fig. 5.
By among Fig. 4 as can be known, two platforms of thermal degradation process experience in the TG curve, first flex point is that wood powder begins to decompose, second flex point is that polypropylene begins to decompose.As seen from Figure 5, the highest decomposition temperature of wood powder moves to low temperature after adding APP and the M-APP, and polyacrylic highest decomposition temperature moves to high temperature.Analyze as can be known, the initial resolving time of wood plastic composite shortens behind adding APP or the M-APP, promotes that matrix material becomes charcoal; Compare with adding APP, add M-APP and make T
1wt%Ease down to 102.3 ℃, T by 110.7
Max1Be reduced to 322.9 ℃, T by 329.3
Max2Bring up to 519.6 ℃ by 518.0, carbon residue brings up to 22.7% by 21.5 in the time of 800 ℃.
The heat release rate (HRR) of the wood powder that the does not add fire retardant/polypropylene wood plastic composite materials of present embodiment-time (s) curve is shown in curve among Fig. 62.
The total heat burst size (THR) of the wood powder that the does not add fire retardant/polypropylene wood plastic composite materials of present embodiment-time (s) curve is shown in curve among Fig. 72.
The total smoke release (TSP) of the wood powder that the does not add fire retardant/polypropylene wood plastic composite materials of present embodiment-time (s) curve is shown in curve among Fig. 82.
Contrast for convenience, with embodiment 16 be that total heat burst size (THR)-time (s) curve, total heat burst size (THR)-time (s) curve and total smoke release (TSP)-time (s) curve of the wood powder/polypropylene wood plastic composite materials of fire retardant is correspondingly charged among Fig. 6, Fig. 7 and Fig. 8 respectively with silane-modified ammonium polyphosphate, be designated as curve 3.
Analysis-by- synthesis contrast embodiment 16,17 and 18 can get, embodiment 17 be that the mechanical property of wood powder/polypropylene wood plastic composite materials of fire retardant is than the poor mechanical property of the wood powder/polypropylene wood plastic composite materials of embodiment 18 with the ammonium polyphosphate, the adding of high polar polymer ammonium polyphosphate is described, its dispersiveness and associativity in wood plastic composite is bad, so the mechanical properties decrease on the contrary of wood powder/polypropylene wood plastic composite materials behind the adding APP.Adopting ammonium polyphosphate after γ-methacryloxypropyl trimethoxy silane modification is that the mechanical property of the wood powder/polypropylene wood plastic composite materials of fire retardant has improved than the mechanical property of the wood powder/polypropylene wood plastic composite materials of embodiment 18, explanation improves with the dispersed and associativity in wood powder/polypropylene wood plastic composite materials of the ammonium polyphosphate after silane modified, consistency improves, and makes the mechanical property of wood powder/polypropylene wood plastic composite materials improve greatly.
Simultaneously the resistance toheat of the wood plastic composite of embodiment 16 and flame retardant properties all improve than the resistance toheat and the flame retardant properties of the wood plastic composite of embodiment 17, improve.
Embodiment 19: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 25g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 0.5g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 24.93MPa, and flexural strength is 61.98MPa, and shock strength is 4.33kJ/m
2
Present embodiment be the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, realize by following steps: one, by weight 100g ammonium polyphosphate, 0.5g γ-methacryloxypropyl trimethoxy silane and 150mL dehydrated alcohol are put into there-necked flask, stir 1h down at 60 ℃, suction filtration then, then filter cake is placed baking oven, under 105 ℃ of conditions, dry 3h, get silane-modified ammonium polyphosphate (M-APP); Two, take by weighing following raw material by weight: silane-modified ammonium polyphosphate, the 6g m-pseudoallyl-α of 60g wood powder, 40g polypropylene, the preparation of 25g step 1, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1g antioxidant 1010; Three, the raw material mixing and stirring that step 2 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that silane-modified ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
Embodiment 20: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 25g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 1.0g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 25.35MPa, and flexural strength is 63.03MPa, and shock strength is 4.45kJ/m
2
Present embodiment be that the preparation method of record in preparation method and the embodiment 19 of wood powder/polypropylene wood plastic composite materials of fire retardant compares with silane-modified ammonium polyphosphate, the consumption difference of γ-methacryloxypropyl trimethoxy silane, all the other steps and parameter are identical in step 1.
Embodiment 21: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 25g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 2.0g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 25.20MPa, and flexural strength is 62.02MPa, and shock strength is 4.11kJ/m
2
Present embodiment be that the preparation method of record in preparation method and the embodiment 19 of wood powder/polypropylene wood plastic composite materials of fire retardant compares with silane-modified ammonium polyphosphate, the consumption difference of γ-methacryloxypropyl trimethoxy silane, all the other steps and parameter are identical in step 1.
Embodiment 22: present embodiment is for being the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is by 60g wood powder, 40g polypropylene, the silane-modified ammonium polyphosphate of 30g (M-APP), 6g m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene (m-TMI-g-PP) coupling agent and 1g antioxidant 1010 are made, and described silane-modified ammonium polyphosphate is made by 100g ammonium polyphosphate and 1.5g γ-methacryloxypropyl trimethoxy silane.
Present embodiment be that the wood powder/polypropylene wood plastic composite materials of fire retardant has that flame retardant properties is good, mechanical property is high, the advantage that resistance toheat is good with silane-modified ammonium polyphosphate.Mechanical property is good, and tensile strength is 26.31MPa, and flexural strength is 62.46MPa, and shock strength is 4.88kJ/m
2
Present embodiment be that the preparation method of record in preparation method and the embodiment 14 of wood powder/polypropylene wood plastic composite materials of fire retardant compares with silane-modified ammonium polyphosphate, the silane-modified ammonium polyphosphate that takes by weighing in step 2 is changed into the 20g, and remaining step and parameter are the same.
Wherein, the data of the mechanical property of the wood plastic composite that relates among the present invention all obtain by following testing method: use omnipotent mechanical test machine to measure the tensile strength and the flexural strength of wood plastic composite, use cantilevered Impact Test machine to measure the shock strength of matrix material.Every kind of sample balance test is averaged for 5 times, and tensile strength is tested according to the ASTMD638 standard, and draw speed is 5mm/min; The flexural strength test is according to ASTM D790 standard, and test speed is 2mm/min, and span is 64mm; The shock strength test is according to ASTM D256 standard.
The data of the resistance toheat of the wood plastic composite that relates among the present invention all obtain by following testing method: use Perkin-Elmer Pyris 1 thermogravimetric analysis instrument that sample is carried out the thermal destruction behavioural analysis, experiment is carried out under the pure nitrogen gas environment, is 10 ℃ of min with temperature rise rate
-1Be raised to 800 ℃ from 30, each example weight is about 3-5mg.
The data of the flame retardant properties of the wood plastic composite that relates among the present invention all obtain by following testing method: the taper calorimeter is tested according to ASTM 1356-90 standard, sample specification is 100 * 100 * 3mm sheet material, adopt FTTStandard taper calorimeter to test, the thermal radiation flow of employing is 50kW/m
2
Claims (10)
1. one kind is the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that with silane-modified ammonium polyphosphate being that the wood powder/polypropylene wood plastic composite materials of fire retardant is by weight by 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of silane-modified ammonium polyphosphates, 3～6 parts of m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 0.1～1 part of oxidation inhibitor are made, and described silane-modified ammonium polyphosphate is to be made by 80～100 parts of ammonium polyphosphates and 0.5～2 part of γ-methacryloxypropyl trimethoxy silane by weight.
2. according to claim 1 a kind of be the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that with silane-modified ammonium polyphosphate be the wood powder/polypropylene wood plastic composite materials of fire retardant by weight by 60 parts of wood powders, 40 parts of polypropylene, 20 parts of silane-modified ammonium polyphosphates, 6 parts of m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor are made.
3. according to claim 1 a kind of be the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that with silane-modified ammonium polyphosphate be the wood powder/polypropylene wood plastic composite materials of fire retardant by weight by 60 parts of wood powders, 40 parts of polypropylene, 25 parts of silane-modified ammonium polyphosphates, 6 parts of m-pseudoallyl-α, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor are made.
According to claim 1,2 or 3 described a kind of be the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that described silane-modified ammonium polyphosphate is to be made by 90～100 parts of ammonium polyphosphates and 1～2 part of γ-methacryloxypropyl trimethoxy silane by weight.
According to claim 1,2 or 3 described a kind of be the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that described silane-modified ammonium polyphosphate is to be made by 100 parts of ammonium polyphosphates and 1.5 parts of γ-methacryloxypropyl trimethoxy silane by weight.
6. as claimed in claim 1 is the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that with silane-modified ammonium polyphosphate being that the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant realizes by following steps: one, by weight with 80～100 parts of ammonium polyphosphates, 0.5～2 parts of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol are put into there-necked flask, stir 1h down at 60 ℃, suction filtration then, then filter cake is placed baking oven, under 105 ℃ of conditions, dry 3h, get silane-modified ammonium polyphosphate, wherein the ratio of ammonium polyphosphate weight and dehydrated alcohol volume is 80～100g: 150mL; Two, take by weighing following raw material by weight: silane-modified ammonium polyphosphate, 3～6 parts of m-pseudoallyl-α of 50～70 parts of wood powders, 30～50 parts of polypropylene, 15～30 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 0.1～1 part of oxidation inhibitor; Three, the raw material mixing and stirring that step 2 is taken by weighing gets compound, then the compound input is had in the feeder of metering, and regulating the feeding rotating speed is 5rmin
-1, and then send in the twin screw extruder, the temperature of each section extruder temperature from the charging opening to the head that twin screw extruder is set is respectively 160 ℃, 170 ℃, 170 ℃, 180 ℃, 180 ℃, 175 ℃, 165 ℃, 160 ℃, and screw speed is 40rmin
-1, the length-to-diameter ratio of twin screw extruder is 35: 1, after compound was extruded by twin screw extruder, cooling promptly was able to the wood powder that silane-modified ammonium polyphosphate is a fire retardant/polypropylene wood plastic composite materials.
7. according to claim 6 is the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that in the step 1 by weight 90～100 parts of ammonium polyphosphates, 1～2 part of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol are put into there-necked flask.
8. according to claim 6 is the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that in the step 1 by weight 100 parts of ammonium polyphosphates, 1.5 parts of γ-methacryloxypropyl trimethoxy silane and dehydrated alcohol are put into there-necked flask.
According to claim 6,7 or 8 described be the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that taking by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 20 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.
According to claim 6,7 or 8 described be the preparation method of the wood powder/polypropylene wood plastic composite materials of fire retardant with silane-modified ammonium polyphosphate, it is characterized in that taking by weighing following raw material in the step 2 by weight: silane-modified ammonium polyphosphate, 6 parts of m-pseudoallyl-α of 60 parts of wood powders, 40 parts of polypropylene, 25 parts of step 1 preparations, α-Er Jiajibianji isocyanic ester graft polypropylene coupling agent and 1 part of oxidation inhibitor.
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| CN109679208A (en) * | 2018-12-14 | 2019-04-26 | 金旸（厦门）新材料科技有限公司 | A kind of environment-friendly high-efficiency anti-flaming polypropylene composite and preparation method thereof |
| US11312862B2 (en) | 2019-08-07 | 2022-04-26 | Dow Silicones Corporation | Solid carrier component including a liquid polydiorganosiloxane and methods for preparation and use of the solid carrier component |
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