CN105566755B - A kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material and its manufacture method - Google Patents

A kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material and its manufacture method Download PDF

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CN105566755B
CN105566755B CN201511033031.8A CN201511033031A CN105566755B CN 105566755 B CN105566755 B CN 105566755B CN 201511033031 A CN201511033031 A CN 201511033031A CN 105566755 B CN105566755 B CN 105566755B
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flame
wood
plastic composite
colloid
composite material
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CN105566755A (en
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梅长彤
潘明珠
徐信武
雍宬
沈梦濛
黄润州
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Nanjing Forestry University
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Nanjing Forestry University
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    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions 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
    • C08L23/10—Homopolymers or copolymers of propene
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • C08L97/00—Compositions of lignin-containing materials
    • C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/24—All layers being polymeric
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    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
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    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
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    • B32B2307/00—Properties of the layers or laminate
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Abstract

The present invention discloses a kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material and its manufacture method.Flame-retardant wood-plastic composite material is watch core Rotating fields, top layer uses polyolefin plastics, wood fibre, nano-meter flame retardantses, lubricant, coupling agent as raw material, and sandwich layer uses polyolefin plastics, wood fibre, crystalline state nanometer cellulose/APP colloid, lubricant, coupling agent as raw material.Raw material passes through in proportion just to be mixed, and top layer raw material is placed in single screw extrusion machine, core layer raw material is placed in double screw extruder, synchronously extrudes, shapes, cools down after fusion plastification, and the flame-retardant wood-plastic composite material of watch core Rotating fields is made.Watch core Rotating fields flame-retardant wood-plastic composite material produced by the present invention has higher fire resistance, mechanical strength, and possesses preferable case hardness, surface rub resistance and anti-fire agent leachability.

Description

A kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material and its manufacture method
Technical field
The invention belongs to the manufacturing field of wood plastic composite, and in particular to a kind of by changing table, sandwich layer fire retardant Component and its adding proportion prepare flame-retardant wood-plastic composite material and its manufacture method.
Background technology
With the continuous expansion of wood plastic composite application field indoors, the research of the fire savety of the composite Using gradually starting to be taken seriously.The anti-flammability of wood plastic composite is mainly by adding the sides such as fire retardant, surface flame-retardant processing Formula assigns.APP is the fire retardant commonly used in wood plastic composite.APP is thermally decomposed to generate polyphosphoric acid and discharged Going out gas, decomposable process heat absorption, so as to reduce the temperature of surrounding, the non-combustible gas discharged waters down air or fuel gas, The material of free radical can be captured by being produced in decomposable process, cut off free radical lock reaction, macromolecule is produced dehydration generation For carbon and water, without producing fuel gas, fire retardation is played in gas phase and solid phase.But there is addition for APP Measure big, susceptible to hydrolysis under the bad border of humidity and be lost in surface migration, cause the reduction of flame retarding efficiency, meanwhile, compound In the preparation process of material, APP is easily reunited, the poor compatibility with composite, causes processing characteristics and the impact of material Performance is decreased obviously.
With the progress of nanosecond science and technology, using nano material as the fire retarding synergist of APP improving polyphosphoric acid Ammonium is above-mentioned to turn into the field developed rapidly in recent years using defect.Publication No. CN 102702767A Chinese patent Disclose one kind and use flame-retardant wood-plastic composite material made from biomass nano silica synergistic APP.However, in reality In the application on border, following three problems are still suffered from：(1) nano material and APP are huge in bulk density and specific surface area Big difference so that both are difficult to be distributed in wood plastic composite system；(2) APP is inorganic substances, with wood plastics composite The interface compatibility of material system is poor；(3) nano material is dispersed in whole system, in combustion, it is necessary to certain Time-shift produces screen effect to system top layer, there is certain hysteresis quality from the point of view of flame retardant effect.If solve simultaneously more than Three problems, then it can greatly promote application of the nano material synergistic APP in flame-retardant wood-plastic composite material.
Cellulose is one of natural polymerses most abundant in nature.Crystalline state nanometer cellulose (nanocrystalline cellulose, NCC) is a kind of a diameter of 1~100nm, the rigidity that length is tens to hundreds of nm Rod-like fibre element.Crystalline state nanometer cellulose possesses the characteristic of high-purity, high-crystallinity, high Young's modulus, high intensity, has simultaneously Multiple reactive hydroxyls are contained on multi-stage artery structure, chiral liquid crystal arrangement, its surface, are easy to be grafted siloxy, amino, absorption Electronics etc., therefore increasingly attracted attention by templated synthesis functional material of crystalline state nanometer cellulose.Publication No. CN 105034108A Chinese patent discloses a kind of side that polymolecularity APP colloid is prepared using crystalline state nanometer cellulose Method, it can greatly improve the dispersiveness of APP and the compatibility with matrix material.
Co-extrusion technology is that one kind is united using two or more extruders by a composite co-extruding head, Extruder is supplied respectively to different fused materials, and continuously extrudes MULTILAYER COMPOSITE product after converging in composite machine head, so as to real Now merging by different top layers and core material, different performances is provided for wood plastic composite.Sandwich layer often provides power Performance is learned, based on common wood moulding or the wood moulding of high filler loading capacity wood fibre, top layer then assigns wood by adding different auxiliary agents The different function of plastic composite materials.Wood plastic composite difference can be assigned by the design of watch core Rotating fields and the change of component Function.
It is domestic at present temporarily have not seen by the design of wood plastic composite watch core Rotating fields and each layer flame retardant compositions and Percentage by weight is adjusted the Patents of flame-retardant wood-plastic composite material are prepared.
The content of the invention
The purpose of the present invention
The present invention provides a kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material, overcomes nano material synergistic APP Existing dispersiveness is bad during flame-retardant wood-plastic composite material, causes with the interface compatibility difference of matrix material and fire retardant loss Poor mechanical property, flame retarding efficiency decline the defects of.
The technical solution of the present invention
Originally the nano material being added in wood plastic composite entirety and APP are distributed to by the present invention respectively to be received In rice crystalline cellulose, nano-meter flame retardantses, crystalline state nanometer cellulose/APP colloid is made, is then respectively added to table, core Coating systems, co-extrusion technology synchronization extrusioning shaping is recycled, flame-retardant wood-plastic composite material is made, its top layer is outer layer, is hindered for nanometer The fire-retardant wood and plastic composite bed of material of agent is fired, thickness is 1.0mm~3.5mm, sandwich layer is internal layer, is crystalline state nanometer cellulose/poly- phosphorus Sour ammongelatine body flame-retardant wood-plastic composite material layer, thickness are 3.5mm~25mm.
A kind of specific preparation method of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material is as follows：
(1) according to the percentage by weight of top layer component, polyolefin plastics 45~70%, wood fibre 5~25% is weighed, is received Rice fire retardant 10~30%, lubricant 1~2%, coupling agent 2~3%,
(2) according to the percentage by weight of sandwich layer component, weigh polyolefin plastics 18~55%, wood fibre 30~65%, Crystalline state nanometer cellulose/APP colloid 5~15%, lubricant 2~3%, coupling agent 2.5~6%；
(3) the above-mentioned nano-meter flame retardantses weighed are sprayed into surface wood fiber surface, then weighed with above-mentioned steps (1) Polyolefin plastics well, lubricant, coupling agent are carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h；
(4) the above-mentioned crystalline state nanometer cellulose/APP colloid weighed is sprayed into sandwich layer wood fibre surface, then Polyolefin plastics, lubricant, the coupling agent weighed with above-mentioned steps (2) carries out just mixed, dry, drying temperature 105 respectively DEG C, drying time 2h；
(5) above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in single screw rod Extruder, barrel zone temperature are 140~220 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, Barrel zone temperature is 155~195 DEG C, and screw speed is 4~6r/min so that raw materials melt plastifies；Then single screw extrusion machine, double The fusion plastification product of screw extruder is synchronous by mould, by mould extrusioning shaping；
(6) cooled down, shaped, cut by mode of traction, flame-retardant wood-plastic composite material is made.
Advantages of the present invention
Watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material prepared by the present invention has higher fire resistance (oxygen index (OI) >=25%, average HRR≤140kW/m2) and higher mechanical strength (bending strength >=25MPa, impact strength >= 18kJ/m2), simultaneously because top layer is the wood and plastic composite bed of material of nano-meter flame retardantses processing, it is compound to be advantageous to raising flame-retardant wood-plastic The hardness and rub resistance of material, and the loss of sandwich layer crystalline state nanometer cellulose/APP is prevented, keep flame retarding efficiency.
Brief description of the drawings
Accompanying drawing 1 is the watch core Rotating fields of flame-retardant wood-plastic composite material.
Embodiment
Embodiment 1, (1) top layer component weigh by weight percentage 67% polypropylene, 10% wood fibre, 20% Crystalline state nanometer cellulose/silicon dioxide colloid (mass fraction of colloid is 35~60%), 1% lubricant, 2% coupling Agent；(2) sandwich layer component weighs 19.5% polyethylene, 65% wood fibre, 10% crystalline state nanometer fibre by weight percentage Tie up element/APP colloid (mass fraction of colloid is 50~75%), 2% lubricant, 3.5% coupling agent；(3) will claim Crystalline state nanometer cellulose/the silicon dioxide colloid taken sprays to surface wood fiber surface, then is weighed with above-mentioned steps (1) Polypropylene, lubricant, coupling agent carry out respectively it is just mixed, dry, drying temperature is 105 DEG C, drying time 2h；(4) will be upper The crystalline state nanometer weighed the cellulose/APP colloid stated sprays to sandwich layer wood fibre surface, then with above-mentioned steps (2) Polyethylene, lubricant, the coupling agent weighed is carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h； (5) above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in single screw extrusion machine, Barrel zone temperature is 200 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, barrel zone temperature 155 DEG C, screw speed is 4~6r/min so that raw materials melt plastifies；Then the melting modeling of single screw extrusion machine, double screw extruder It is synchronous by mould to change product, by mould extrusioning shaping；(6) cooled down, shaped, cut by mode of traction, flame-retardant wood-plastic is made Composite.After tested, the flame-retardant wood-plastic composite material oxygen index (OI) being prepared is 28.2%, HRR 138.1kW/ m2, bending strength 25.7MPa, impact strength 19.6kJ/m2。
Embodiment 2, (1) top layer component weigh by weight percentage 66% polystyrene, 5% wood fibre, 25% Crystalline state nanometer cellulose/nanometer magnesium hydroxide colloidal (mass fraction of colloid be 35~60%), 1% lubricant, 3% Coupling agent；(2) sandwich layer component weighs 18% polyethylene, 60% wood fibre, 15% crystalline state nanometer by weight percentage Cellulose/APP colloid (mass fraction of colloid is 50~75%), 2.5% lubricant, 4.5% coupling agent；(3) The crystalline state nanometer cellulose/nanometer magnesium hydroxide colloidal weighed is sprayed into surface wood fiber surface, then with above-mentioned steps (1) polystyrene, lubricant, the coupling agent weighed carry out respectively it is just mixed, dry, drying temperature is 105 DEG C, and drying time is 2h；(4) the above-mentioned crystalline state nanometer weighed cellulose/APP colloid is sprayed into sandwich layer wood fibre surface, then with Polyethylene that above-mentioned steps (2) have weighed, lubricant, coupling agent carry out respectively it is just mixed, dry, drying temperature is 105 DEG C, is dried Time is 2h；(5) above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in single spiral shell Bar extruder, barrel zone temperature are 220 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, machine barrel Temperature is 165 DEG C, and screw speed is 4~6r/min so that raw materials melt plastifies；Then single screw extrusion machine, twin-screw extrusion The fusion plastification product of machine is synchronous by mould, by mould extrusioning shaping；(6) cooled down, shaped, cut by mode of traction, made Into flame-retardant wood-plastic composite material.After tested, the flame-retardant wood-plastic composite material oxygen index (OI) being prepared is 25%, HRR is 125.7kW/m2, bending strength 30.9MPa, impact strength 18.5kJ/m2。
Embodiment 3, (1) top layer component weigh by weight percentage 60% polyethylene, 5% wood fibre, 30% Crystalline state nanometer cellulose/nanometer montmorillonite colloid (mass fraction of colloid is 35~60%), 2% lubricant, 3% coupling Agent；(2) sandwich layer component weighs 25% polyethylene, 54% wood fibre, 15% crystalline state nanometer fiber by weight percentage Element/APP colloid (mass fraction of colloid is 50~75%), 3% lubricant, 3% coupling agent；(3) will weigh Crystalline state nanometer cellulose/nanometer montmorillonite colloid spray to surface wood fiber surface, then weighed with above-mentioned steps (1) Polyethylene, lubricant, coupling agent are carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h；(4) will be above-mentioned The crystalline state nanometer weighed cellulose/APP colloid spray to sandwich layer wood fibre surface, then claim with above-mentioned steps (2) Polyethylene, lubricant, the coupling agent taken is carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h；(5) Above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in single screw extrusion machine, machine barrel Temperature is 140 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, and barrel zone temperature is 165 DEG C, Screw speed is 4~6r/min so that raw materials melt plastifies；Then the fusion plastification of single screw extrusion machine, double screw extruder Product is synchronous by mould, by mould extrusioning shaping；(6) cooled down, shaped, cut by mode of traction, flame-retardant wood-plastic is made and answers Condensation material.After tested, the flame-retardant wood-plastic composite material oxygen index (OI) being prepared is 26.8%, HRR 135kW/m2、 Bending strength 32.3MPa, impact strength 19.3kJ/m2。
Embodiment 4, (1) top layer component weigh by weight percentage 70% polyethylene, 5% wood fibre, 20% Crystalline state nanometer cellulose/carbon nano colloid (mass fraction of colloid is 35~60%), 2% lubricant, 3% coupling Agent；(2) sandwich layer component weighs 25% polyvinyl chloride, 61% wood fibre, 5% crystalline state nanometer fiber by weight percentage Element/APP colloid (mass fraction of colloid is 50~75%), 3% lubricant, 6% coupling agent；(3) will weigh Crystalline state nanometer cellulose/carbon nano colloid spray to surface wood fiber surface, then weighed with above-mentioned steps (1) poly- Ethene, lubricant, coupling agent are carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h；(4) will be above-mentioned Crystalline state nanometer cellulose/APP the colloid weighed sprays to sandwich layer wood fibre surface, then is weighed with above-mentioned steps (2) Polyvinyl chloride well, lubricant, coupling agent are carried out just mixing respectively, dried, and drying temperature is 105 DEG C, drying time 2h；(5) Above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in single screw extrusion machine, machine barrel Temperature is 140 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, and barrel zone temperature is 165 DEG C, Screw speed is 4~6r/min so that raw materials melt plastifies；Then the fusion plastification of single screw extrusion machine, double screw extruder Product is synchronous by mould, by mould extrusioning shaping；(6) cooled down, shaped, cut by mode of traction, flame-retardant wood-plastic is made and answers Condensation material.After tested, the flame-retardant wood-plastic composite material oxygen index (OI) being prepared is 25.3%, HRR 135.6kW/ m2, bending strength 27.1MPa, impact strength 18.2kJ/m2。

Claims (2)

1. a kind of watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material, it is characterised in that the structure of flame-retardant wood-plastic composite material is table Core structure, top layer are that outer layer is the fire-retardant wood and plastic composite bed of material of nano-meter flame retardantses, and thickness is 1.0mm~3.5mm；Sandwich layer is Internal layer is crystalline state nanometer cellulose/APP colloid flame-retardant wood-plastic composite material layer, and thickness is 3.5mm~25mm；
(1) percentage by weight of top layer component is as follows：Polyolefin plastics 45~70%, wood fibre 5~25%, nano-meter flame retardantses 10~30%, lubricant 1~2%, coupling agent 2~3%,
(2) percentage by weight of sandwich layer component is as follows：Polyolefin plastics 18~55%, wood fibre 30~65%, crystalline state nanometer Cellulose/APP colloid 5~15%, lubricant 2~3%, coupling agent 2.5~6%；
The polyolefin plastics of the top layer and sandwich layer is a kind of or several in polyethylene, polypropylene, polyvinyl chloride, polystyrene The mixture of kind；
The wood fibre of the top layer and sandwich layer is one or several kinds of mixing in timber, rice straw, wheat straw, sawdust, rice husk Thing, particle diameter are 30~100 mesh；
The nano-meter flame retardantses on the top layer are crystalline state nanometer cellulose/silicon dioxide colloid, crystalline state nanometer cellulose/nanometer hydrogen-oxygen Change colloidal magnesium, crystalline state nanometer cellulose/nanometer alumine hydroxide colloid, crystalline state nanometer cellulose/nanometer montmorillonite colloid, nanocrystalline One or several kinds of mixtures in state cellulose/carbon nano colloid, the mass fraction of colloid is 35~60%；
Crystalline state nanometer cellulose/APP colloid of the sandwich layer, the mass fraction of colloid is 50~75%；
The lubricant of the top layer and sandwich layer is a kind of or several in stearic acid, paraffin, talcum powder, calcium carbonate, Tissuemat E The mixture of kind；
The coupling agent of the top layer and sandwich layer be maleic anhydride grafted polyethylene, maleic anhydride inoculated polypropylene, silane coupler, One or several kinds of mixtures in carbonic ester coupling agent.
A kind of 2. watch core layer synchronization co-extrusion flame-retardant wood-plastic composite material according to claim 1, it is characterised in that fire-retardant wood The synchronous extrusion of plastic composite materials watch core layer, step include：
(1) according to the percentage by weight of top layer component, polyolefin plastics 45~70%, wood fibre 5~25%, nanometer resistance are weighed Agent 10~30%, lubricant 1~2%, coupling agent 2~3% are fired,
(2) according to the percentage by weight of sandwich layer component, polyolefin plastics 18~55%, wood fibre 30~65%, nanometer are weighed Crystalline cellulose/APP colloid 5~15%, lubricant 2~3%, coupling agent 2.5~6%；
(3) according to top layer component, the above-mentioned nano-meter flame retardantses weighed are sprayed into surface wood fiber surface, then with weighing Polyolefin plastics, lubricant, coupling agent carry out respectively it is just mixed, dry, drying temperature is 105 DEG C, drying time 2h；
(4) according to sandwich layer component, the above-mentioned crystalline state nanometer cellulose/APP colloid weighed is sprayed into the wooden fibre of sandwich layer Dimension table face, then polyolefin plastics, lubricant, coupling agent with having weighed are carried out just mixing respectively, dried, and drying temperature is 105 DEG C, Drying time is 2h；
(5) above-mentioned dried mixture is respectively placed in extruder hopper, wherein, overlay mixture is placed in Single screw extrusion Machine, barrel zone temperature are 140~220 DEG C, and screw speed is 5~12r/min, and sandwich layer mixture is placed in double screw extruder, machine barrel Temperature is 155~195 DEG C, and screw speed is 4~6r/min so that raw materials melt plastifies；Then single screw extrusion machine, twin-screw The fusion plastification product of extruder is synchronous by mould, by mould extrusioning shaping；
(6) cooled down, shaped, cut by mode of traction, flame-retardant wood-plastic composite material is made.
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