CN110003677A - A kind of halogen-free polypropylene flame redardant wood plastic composite and preparation method thereof - Google Patents
A kind of halogen-free polypropylene flame redardant wood plastic composite and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- C08K2003/0856—Iron
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of halogen-free polypropylene flame redardant wood plastic composite and preparation method thereof, each component including following mass fraction: 10-50 parts of waste epoxy resin, 20-60 parts of polypropylene, 20-60 parts of wood powder, 15-40 parts of flame-retardant system, 10-40 parts of antistatic agent, 2-10 parts of coupling agent, 5-15 parts of expanding material, 2-5 parts of heat stabilizer, 1-4 parts of antioxidant, 1-4 parts of lubricant.The present invention prepares wood plastic composite with " two step fusion methods ", and this method can be effectively improved interface compatibility, and the flame retardant effect of wood plastic composite is improved under the premise of keeping excellent mechanical performances.Polypropylene wood-plastic composite material prepared by the present invention has production procedure simple, and flame retardant effect is good, can efficiently reduce environmental pollution while realizing that waste epoxy resin recycles, protect forest resources.
Description
Technical field
The present invention relates to a kind of wood plastic composite and preparation method thereof, specifically a kind of halogen-free polypropylene flame redardant wood
Plastic composite materials and preparation method thereof.
Background technique
Wood plastic composite (Wood Plastic Composite, WPC) is by low cost, natural timber, Ma Dengtian
Right fiber or powder body material and thermoplastic (including PE, PP, PVC etc.) are a kind of compounded green ring of primary raw material
It protects, environmental-friendly new material.WPC has good processing performance and mechanical performance, and market potential is huge.In recent years,
With greatly developing for electronics industry, epoxy resin is widely used in because of its good electrical insulation capability and sealing performance
The shell of electronic product.However, epoxy resin because of its special tridimensional network and insoluble characteristic, is difficult to utilize again.It will
It is added in high-molecular organic material by the waste epoxy resin that Mechanical Crushing obtains as filler and regeneration high molecular material is made,
The cost of product can not only be reduced, moreover it is possible to alleviate waste landfill and burn brought environmental pressure.Further, since wooden fibre
Dimension, plastics are hydrocarbon, and Wood-plastic material is meeting open fire or in case of heating equal incendivity, and is difficult certainly after burning
It puts out, therefore WPC is to be difficult to reach the requirement of code for fire prevention design of interior decoration of buildings without flame retardant treatment, is not allowed in principle
It is directly used as related constructional ornamental material.
Improve the flame retardant property of wood plastic composite by addition fire retardant mostly both at home and abroad at present.Application No. is
A kind of high-strength anti-flaming Wood-plastic material of 201811153485.2 patent disclosure and preparation method thereof, discovery pass through three oxygen of addition
Change two antimony (Sb2O3) it can significantly improve the flame retardant property of the Wood-plastic material, but Sb2O3It is defended in October, 2017 by the world
Raw tissue (WHO) is classified as 2B class carcinogenic substance inventory, has harmfulness for human body health.Application No. is
A kind of polypropylene flame redardant sill plastic composite board of 201810046114.8 patent disclosure and preparation method, however its fire-retardant changes
Property complex process, it is at high cost, it is unfavorable for industrialized production.Application No. is the patent disclosure of 201010235935.X is a kind of fire-retardant
Wood plastic composite and preparation method thereof, it carries out wood plastic composite by the red phosphorus that addition mass fraction is 2%-10%
It is fire-retardant, obtain preferable flame retardant effect, however red phosphorus itself is easy to moisture absorption, thermostabilization is poor, when processing extremely toxic phosphatization easily generated
Hydrogen (PH3), cause its application limited.Deka(Journal of Applied Polymer Science,2012,124(4):
It 2919-2929) is prepared for Polyethylene wood plastic composite material, it is found that the anti-flammability of Wood-plastic material can be improved in nanoclay and ZnO
Can, but the flame retarding efficiency for only adding a small amount of clay and ZnO is not high, and excessive addition can reduce the mechanical property of Wood-plastic material
Energy.A kind of preparation method of high-strength anti-flaming PE Wood-plastic floor of 201711279323.9 patent disclosure passes through addition self-control
Flame retarding function mother liquor PE Wood-plastic floor is carried out fire-retardant, flame retardant effect is good, but its disclosed fire retardant preparation process is multiple
It is miscellaneous and at high cost, it is unfavorable for the industrialized production of flame-retardant wood-plastic.
In addition, extremely easy to produce static electricity when in use, electrostatic interaction can make because wood fibre and plastics are insulating properties substance
Product adsorbs the dust in air, is easy to cause precision instrument to be distorted, electronic component failure, What is more, and electrostatic can cause fire
Calamity or generation explosion etc..Application No. is 201711315715.6 patents to disclose a kind of antistatic PVC wood plastic composite material
And preparation method thereof, use the Graphene powder of stratiform as PVC wood plastic composite material items mechanical performance made from antistatic agent
It is excellent, and there is good antistatic property.Application No. is 201410723764.3 patent disclose it is a kind of conductive/antistatic
Polyethylene wood plastic composite material and preparation method thereof, the antistatic agent used are diameter 20-100nm, 10-50 μm of length more
Wall carbon nano tube, prepared Wood-plastic material antistatic effect are good.However, antistatic agent price used in above method is high
It is expensive, cause the production cost of antistatic wood plastic composite excessively high, is unfavorable for realizing industrialized production.
Summary of the invention
The present invention is poor in order to solve existing wood plastic composite fire protecting performance, and antistatic is at high cost and is unfavorable for industrial metaplasia
The problems such as production, discloses a kind of halogen-free polypropylene flame redardant wood plastic composite and preparation method thereof.
The present invention is blended with waste epoxy resin with thermoplastic, then compound with wood powder, and ammonium polyphosphate (APP) is fire-retardant
Agent, iron powder are antistatic agent, prepare wood plastic composite by two step melting extrusion techniques.Due to being pre-processed to wood powder
With using second melting technique, the interfacial bond property between resin and wood fibre and blending resin is effectively improved,
And improve the impact flexibility of composite material.Moreover, the present invention is while realizing waste epoxy resin recycling and reusing, effectively
Ground reduces environmental pollution, constructs resource-conserving and environment-friendly society for China and provides the approach of a sustainable development.
Halogen-free polypropylene flame redardant wood plastic composite of the present invention is obtained by major ingredient and auxiliary material processing.
The major ingredient includes each component of following mass parts:
10-50 parts of waste epoxy resin
20-60 parts of thermoplastic
20-60 parts of wood powder.
The auxiliary material includes each component of following mass parts:
The waste epoxy resin is the waste epoxy resin powder after crushing, milling, be sieved, partial size 40-100
Mesh.
The thermoplastic is polypropylene (PP), and the polyacrylic melt flow rate (MFR) is 0.5-5g/10min.
The partial size of the wood powder is 40-80 mesh.
The flame-retardant system includes fire retardant and synergist, and wherein fire retardant is the ammonium polyphosphate of degree of polymerization 1000-4000,
Synergist is one or more of pentaerythrite, melamine, magnesium hydroxide, aluminium hydroxide etc.；It is hindered in the flame-retardant system
The mass ratio for firing agent and synergist is 1:2-4:1.
The antistatic agent is one or more of in the metal powders such as iron powder, copper powder, aluminium powder；And the partial size of metal powder exists
20-100μm。
The coupling agent is silane coupling agent, aluminate coupling agent, zirconium ester coupling agent, titanate coupling agent, phosphorous idol
Join any one in agent etc..
The expanding material connects polypropylene (MAH-g-PP) for maleic anhydride branch, and grafting rate >=0.8% of MAH.
The heat stabilizer is Ca-Zn composite heat stabilizer, and effect is to play heat stabilization to blending resin.
Any one of the antioxidant in Hinered phenols, phosphorous acid esters, thioesters, composite antioxidant etc..
The lubricant is selected from atoleine, stearic acid, calcium stearate, zinc stearate, ethlyene dichloride wax, ethylene oxide wax
In any one.
Further, the mass ratio of the waste epoxy resin and thermoplastic is 1:1-1:3.
Further, the mass ratio of the coupling agent and wood powder is 1:10-1:20.
The preparation method of halogen-free polypropylene flame redardant wood plastic composite of the present invention, includes the following steps:
Step 1: the drying of waste epoxy resin and wood powder
Waste epoxy resin, wood powder are dried into 4-8h in 60-90 DEG C of baking oven, make its moisture content lower than 2%；
Step 2: the pretreatment of wood powder
Wood powder is immersed in the ethyl alcohol containing coupling agent, ultrasonic disperse 1-3h, heating stirring is put into baking oven to solidifying
Dry 1-2h obtains pretreatment wood powder；
Step 3: a melting mixing and extruding pelletization
Waste epoxy resin, thermoplastic, antistatic agent, expanding material, heat stabilizer, antioxidant and lubricant are added
Mixed once material is uniformly mixing to obtain to high-speed mixer；Mixed once material is added twin-screw extrude, is carried out for the first time
Melt blending, extruding pelletization obtain pellet A；
Step 4: second melting mixing and extrusion molding
Pellet A and pretreatment wood powder, fire retardant and synergist are added in high-speed mixer and are uniformly mixed to obtain two
Secondary mixture；Secondary mixed material is added twin-screw extrude, second of melt blending is carried out, it is poly- to squeeze out obtained halogen-free flameproof
Propylene wood plastic composite.
In step 3, the temperature of high-speed mixer is set as 40-60 DEG C, revolving speed 300-500rpm, incorporation time 10-
20min。
In step 3, the extrusion temperature of double screw extruder is 190-215 DEG C, screw speed 80-120rpm.
In step 4, the temperature of high-speed mixer is set as 40-60 DEG C, revolving speed 300-500rpm, incorporation time 10-
20min。
In step 4, the extrusion temperature of double screw extruder is 185-210 DEG C, screw speed 70-110rpm.
The present invention prepares wood plastic composite with " melting of two steps " technique, and it is compatible that this method can effectively improve interface
Property, prepared composite material can have good flame retardant property and antistatic under the premise of keeping good mechanical properties
Performance.Technical process of the invention is simple, is advantageously implemented industrialized production.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of 1 sample in cross section of embodiment.
Fig. 2 is the stereoscan photograph of 2 sample in cross section of embodiment.
Fig. 3 is the stereoscan photograph in comparative example section.
Specific embodiment
The present invention is further illustrated below with reference to specific embodiment, but the scope of the present invention is not by these embodiments
Limitation.
Embodiment 1:
1, ingredient
Waste epoxy resin: 300g
PP plastics: 300g
Wood powder: 600g
APP:150g
Mg(OH)2: 50g
Fe powder: 150g
Aluminate coupling agent: 70g
MAH-g-PP:50g
Calcium zinc heat stabilizer: 20g
Irgasfos 168: 20g
Stearic acid: 15g
2, it prepares
(1) waste epoxy resin, wood powder are dried to 5h in 80 DEG C of baking ovens, make its moisture content lower than 2%；
(2) wood powder is immersed in the ethyl alcohol containing aluminate coupling agent, after ultrasonic disperse 2h, heating stirring to solidification,
It is placed in oven and dried 1h；
(3) by waste epoxy resin, PP plastics, Fe powder, MAH-g-PP, calcium zinc heat stabilizer, irgasfos 168 and stearic acid
It is added in high-speed mixer, mixes 15min under the conditions of 40 DEG C, revolving speed 400rpm, obtain mixed once material A；Mixed once
Material A is added twin-screw extrude and is carried out first time melt blending, granulation obtains pellet A, and extrusion temperature is 210 DEG C, and screw rod turns
Speed is 120rpm；
(4) by above-mentioned pellet A and pretreated wood powder, APP and Mg (OH)2It is added in high-speed mixer, in 40 DEG C, turns
15min is mixed under the conditions of fast 400rpm, obtains secondary mixed material；Secondary mixed material is added twin-screw extrude, in temperature
205 DEG C, under the conditions of screw speed 105rpm, carry out second of melt blending, squeeze out and halogen-free polypropylene flame redardant wood plastics composite be made
Material.
Embodiment 2:
1, ingredient
Waste epoxy resin: 180g
PP plastics: 420g
Wood powder: 600g
APP:150g
Mg(OH)2: 50g
Fe powder: 150g
Aluminate coupling agent: 70g
MAH-g-PP:50g
Calcium zinc heat stabilizer: 20g
Irgasfos 168: 20g
Stearic acid: 15g
2, it prepares
(1) waste epoxy resin, wood powder are dried to 5h in 80 DEG C of baking ovens, make its moisture content lower than 2%；
(2) wood powder is immersed in the ethyl alcohol containing aluminate coupling agent, after ultrasonic disperse 2h, heating stirring to solidification,
It is placed in oven and dried 1h；
(3) by waste epoxy resin, PP plastics, Fe powder, MAH-g-PP, calcium zinc heat stabilizer, irgasfos 168 and stearic acid
It is added in high-speed mixer, mixes 15min under the conditions of 40 DEG C, revolving speed 400rpm, obtain mixed once material A；Primary mixed
It closes and expects that A adds twin-screw extrude progress first time melt blending, granulation obtains pellet A, extrusion temperature is 210 DEG C, screw rod
Revolving speed is 120rpm；
(4) by above-mentioned pellet A and pretreated wood powder, APP and Mg (OH)2It is added in high-speed mixer, in 40 DEG C, turns
15min is mixed under the conditions of fast 400rpm, obtains secondary mixed material；Secondary mixed material is added twin-screw extrude, in temperature
205 DEG C, under the conditions of screw speed 105rpm, carry out second of melt blending, squeeze out and halogen-free polypropylene flame redardant wood plastics composite be made
Material.
Comparative example:
1, ingredient
Waste epoxy resin: 300g
PP plastics: 300g
Wood powder: 600g
Aluminate coupling agent: 70g
MAH-g-PP:50g
Calcium zinc heat stabilizer: 20g
Irgasfos 168: 20g
Stearic acid: 15g
2, it prepares
(1) waste epoxy resin, wood powder are dried to 5h in 80 DEG C of baking ovens, make its moisture content lower than 2%；
(2) wood powder is immersed in the ethyl alcohol containing aluminate coupling agent, after ultrasonic disperse 2h, heating stirring to solidification,
It is placed in oven and dried 1h；
(3) waste epoxy resin, PP plastics, MAH-g-PP, calcium zinc heat stabilizer, irgasfos 168 and stearic acid are added
Into high-speed mixer, 15min is mixed under the conditions of 40 DEG C, revolving speed 400rpm, obtains mixed once material A；Mixed once material A
It adds twin-screw extrude and carries out first time melt blending, be granulated and obtain pellet A, extrusion temperature is 210 DEG C, and screw speed is
120rpm；
(4) above-mentioned pellet A and wood powder are added in high-speed mixer, are mixed under the conditions of 40 DEG C, revolving speed 400rpm
15min obtains secondary mixed material；Secondary mixed material is added twin-screw extrude, in 205 DEG C of temperature, screw speed
Under the conditions of 105rpm, second of melt blending is carried out, squeezes out and halogen-free polypropylene flame redardant wood plastic composite is made.
The composite material of embodiment and comparative example preparation is subjected to combustibility, antistatic property and Mechanics Performance Testing.
As a result as follows:
The performance test parameter list of table 1.PP wood plastic composite
| Combustion parameter | Embodiment 1 | Embodiment 2 | Comparative example |
| Thermal decomposition temperature (DEG C) | 477.3 | 478.6 | 472.9 |
| Burning time (s) | 31 | 32 | 26 |
| Fall time (s) | 300 | 331 | 336 |
| Total heat discharges (MJ/m2) | 64.5 | 66.0 | 69.6 |
| Rate of heat release mean value (kW/m2) | 239.7 | 220.8 | 224.5 |
| Rate of heat release peak value (kW/m2) | 375.2 | 384.6 | 504.2 |
| Mass loss rate mean value (g/s) | 0.072 | 0.062 | 0.071 |
| Mass loss rate peak value (g/s) | 0.267 | 0.275 | 0.867 |
| The yield mean value (kg/kg) of CO | 0.001 | 0.001 | 0.002 |
| CO2Yield mean value (kg/kg) | 1.141 | 1.692 | 2.120 |
| Charring rate (%) | 29.2 | 27.9 | 26.7 |
| Volume resistivity (Ω m) | 4.13E+07 | 3.94E+07 | 1.19E+08 |
| Notch impact strength (kJ/m2) | 4.5 | 4.9 | 3.9 |
Note: taper calorimetric test is executed according to ASTM E1354,5560 ISO standard；Volume resistivity is according to GB/T
1410-2006 standard testing；Notch impact strength is according to GB/T 1043.1-2008 standard testing.
As known from Table 1, the total Heat liberation unit of comparative example (being not added with fire retardant) and rate of heat release peak value are up to 69.6MJ/
m2、224.5MJ/m2, and after fire retardant is added, the Heat liberation unit and rate of heat release of embodiment 1 and embodiment 2 significantly reduce.This
Outside, the CO of composite material, CO2Yield declined, charring rate is risen, and shows that wood moulding that present implementation obtains is multiple
Condensation material has good flame-retarding characteristic.Be added antistatic agent Fe after, the volume resistivity of embodiment 1,2 relative to comparative example all
An order of magnitude is had dropped, the antistatic property of material is effectively improved.Fig. 1-3 is the scanning electron microscope of three kinds of samples
Photo.It is not difficult to find out that prepared by pretreatment and " melting of two steps " technique by wood powder in sample, wood powder particle and polyphosphoric acid
Ammonium APP particle present well it is uniformly dispersed, be effectively facilitated filler and be rationally scattered on phase interface, realize impact strength
Raising.
In summary, the present invention can keep wood plastic composite fire-retardant under the premise of guaranteeing has good mechanical properties
Performance and antistatic property are improved significantly simultaneously, and technical process is simple, are suitble to industrialized production.
Illustrative description only is done to the present invention above, it should be noted that the case where not departing from core of the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Within the scope of the present invention.
Claims (10)
1. a kind of halogen-free polypropylene flame redardant wood plastic composite, it is characterised in that the halogen-free polypropylene flame redardant wood plastic composite
It is obtained by major ingredient and auxiliary material processing；
The major ingredient includes each component of following mass parts:
10-50 parts of waste epoxy resin
20-60 parts of thermoplastic
20-60 parts of wood powder；
The auxiliary material includes each component of following mass parts:
2. halogen-free polypropylene flame redardant wood plastic composite according to claim 1, it is characterised in that:
The waste epoxy resin is the waste epoxy resin powder after crushing, milling, be sieved, and partial size is 40-100 mesh；
The thermoplastic is polypropylene, and the polyacrylic melt flow rate (MFR) is 0.5-5g/10min；
The partial size of the wood powder is 40-80 mesh.
3. halogen-free polypropylene flame redardant wood plastic composite according to claim 1, it is characterised in that:
The flame-retardant system includes fire retardant and synergist, and wherein fire retardant is the ammonium polyphosphate of degree of polymerization 1000-4000, synergistic
Agent is one or more of pentaerythrite, melamine, magnesium hydroxide, aluminium hydroxide etc.；Fire retardant in the flame-retardant system
Mass ratio with synergist is 1:2-4:1；
The antistatic agent is one or more of in the metal powders such as iron powder, copper powder, aluminium powder, and the partial size of metal powder is in 20-
100μm；
The coupling agent is silane coupling agent, aluminate coupling agent, zirconium ester coupling agent, titanate coupling agent, phosphorous coupling agent
Any one in；
The expanding material is maleic anhydride inoculated polypropylene MAH-g-PP, and grafting rate >=0.8% of MAH；
The heat stabilizer is Ca-Zn composite heat stabilizer；
Any one of the antioxidant in Hinered phenols, phosphorous acid esters, thioesters, composite antioxidant etc.；
The lubricant is in atoleine, stearic acid, calcium stearate, zinc stearate, ethlyene dichloride wax, ethylene oxide wax
Any one.
4. halogen-free polypropylene flame redardant wood plastic composite according to claim 1, it is characterised in that:
The mass ratio of the waste epoxy resin and thermoplastic is 1:1-1:3.
5. halogen-free polypropylene flame redardant wood plastic composite according to claim 1, it is characterised in that:
The mass ratio of the coupling agent and wood powder is 1:10-1:20.
6. the preparation method of any halogen-free polypropylene flame redardant wood plastic composite in a kind of claim 1-5, it is characterised in that
Include the following steps:
Step 1: the drying of waste epoxy resin and wood powder
Waste epoxy resin, wood powder are dried into 4-8h in 60-90 DEG C of baking oven, make its moisture content lower than 2%；
Step 2: the pretreatment of wood powder
Wood powder is immersed in the ethyl alcohol containing coupling agent, ultrasonic disperse 1-3h, heating stirring is placed in oven and dried to solidifying
1-2h obtains pretreatment wood powder；
Step 3: one time melting mixing squeezes out
High speed is added in waste epoxy resin, thermoplastic, antistatic agent, expanding material, heat stabilizer, antioxidant and lubricant
Mixing machine is uniformly mixing to obtain mixed once material；Mixed once material is added twin-screw extrude, melt for the first time altogether
Mixed, pellet A is made in extruding pelletization；
Step 4: second melting mixing squeezes out
Pellet A and pretreatment wood powder, fire retardant and synergist are added in high-speed mixer and are uniformly mixed to obtain secondary mix
Close material；Secondary mixed material is added twin-screw extrude, second of melt blending is carried out, squeezes out and halogen-free polypropylene flame redardant is made
Wood plastic composite.
7. preparation method according to claim 6, it is characterised in that:
In step 3, the temperature of high-speed mixer is set as 40-60 DEG C, revolving speed 300-500rpm, incorporation time 10-20min.
8. preparation method according to claim 6, it is characterised in that:
In step 3, the extrusion temperature of double screw extruder is 190-215 DEG C, screw speed 80-120rpm.
9. preparation method according to claim 6, it is characterised in that:
In step 4, the temperature of high-speed mixer is set as 40-60 DEG C, revolving speed 300-500rpm, incorporation time 10-20min.
10. preparation method according to claim 6, it is characterised in that:
In step 4, the extrusion temperature of double screw extruder is 185-210 DEG C, screw speed 70-110rpm.
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| CN111253659A (en) * | 2020-01-15 | 2020-06-09 | 安捷包装（苏州）股份有限公司 | Production process of long fiber composite board for packing box |
| CN111454485A (en) * | 2020-03-30 | 2020-07-28 | 嘉兴学院 | Antistatic wood-plastic composite material and preparation method thereof |
| CN111925579A (en) * | 2020-07-12 | 2020-11-13 | 武汉柒合兴制造有限公司 | Wood-plastic board processing technology |
| CN112646384A (en) * | 2020-12-19 | 2021-04-13 | 界首市成铭塑业有限公司 | Waste plastic particle modified flame-retardant sheet and preparation method thereof |
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| CN114685895A (en) * | 2022-04-21 | 2022-07-01 | 河北工程大学 | Flame-retardant aging-resistant wood-plastic composite material and preparation method thereof |
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