CN106243471B - A kind of fire-retardant wood-fibred enhancing polyethylene flexible web and its manufacturing method - Google Patents
A kind of fire-retardant wood-fibred enhancing polyethylene flexible web and its manufacturing method Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/08—Conditioning or physical treatment of the material to be shaped by using wave energy or particle radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2497/00—Characterised by the use of lignin-containing materials
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a kind of fire-retardant wood-fibred enhancing polyethylene flexible webs and its manufacturing method, the manufacturing method to include the following steps：Wood-fibred is bleached with degreasing bleaching liquid, wood-fibred, high polymerization degree APP, precipitated calcium carbonate, silane coupling A 172, chlorinated paraffin, dioctyl phthalate and stearic acid after degreasing is bleached are kneaded uniformly in high speed mixing smelting machine, obtain premix；The melmac for spraying into atomization under stirring into premix coats premix；Premix after cladding is dried, the premix after then coating dry melmac is kneaded uniformly with linear low density polyethylene resin, obtains mixture；Mixture is enhanced into polyethylene flexible web by mediating extrusion, mill tabletting, press polish overlay film, molding cooling and shaping and cutting deburring to get fire-retardant wood-fibred successively.Fire-retardant wood-fibred enhancing polyethylene flexible web fire retardant performance is good, intensity is big, flexibility is good for this.
Description
Technical field
The invention belongs to wood plastic composite technical field more particularly to a kind of fire-retardant wood-fibred enhancing polyethylene flexibility volumes
Material and its manufacturing method.
Background technology
Polyethylene (polyethylene, abbreviation PE) is a kind of aggregated thermoplastic resin obtained of ethylene.Polyethylene without
Smelly, nontoxic, feel ceraceous has excellent resistance to low temperature (reachable -100 DEG C~-70 DEG C of minimum temperature in use), chemical stabilization
Property is good, is resistant to the erosion of most of soda acids.Common solvent is not dissolved under room temperature, water imbibition is small, and electrical insulating property is excellent.
Wood-fibred has relatively high strength and stiffness and lower density, is added to polyvinyl chloride, polyethylene, poly- third
Wood plastic composite is made in the plastics such as alkene, ABS resin and polystyrene, there is filling, enhancing to plastics, reduce weight, drop
The effect of low cost.
The advantages of wood plastic composite set timber and plastics, good stability of the dimension is corrosion-resistant, resistance to damage by worms, ageing-resistant,
Recyclable recycling.Wood plastic composite is widely used to the fields such as building, ship vehicle, furniture decoration, is the family of the mankind
It occupies life and provides colourful material selection.
But the shortcomings that wood plastic composite, which is them, has combustibility.It is not only generated when wood plastic composite burns big
Calorimetric, while also discharging a large amount of cigarette and toxic gas.In order to reduce fire hazard, China's pressure from 1 day July in 2008 is held
Row standard GB/T 20286-2006《Public place fire-retardant product and component combustibility require and mark》.According to the standard,
General floorings, furniture and home decoration material will must not be used for the decoration and finishing of public place.Therefore, for often exposing
The home decorations material such as wood-plastic composite floor carry out fire-retardant fireproof processing and be very important.
It is and lipophilic in addition, the inorganic fillers such as hydrophilic wood-fibred, fire retardant and calcium carbonate in wood plastic composite
Interface is incompatible between plastics, causes the reunion of wood-fibred and plastics that cannot effectively be bonded with filler, causes the mechanics of material
Performance declines.The interface compatibility difference of wood-fibred and inorganic filler and plastics is the important of restriction wood plastic composite performance
Factor.Therefore, develop that a kind of fire retardant performance is good, wood plastic composite of good mechanical performance has much realistic meaning.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The fire-retardant wood-fibred enhancing polyethylene flexible web and its manufacturer that kind fire retardant performance is good, mechanical strength is big, flexibility is good
Method.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of fire-retardant wood-fibred enhancing polyethylene flexible web, includes the component of following parts by weight：Linear low density polyethylene
50-60 parts of olefine resin, 40-60 parts of wood-fibred, 8-10 parts of high polymerization degree APP, 80-100 parts of precipitated calcium carbonate, silane are even
Join 2-3 parts of agent A-172,10-12 parts of chlorinated paraffin, 5-26 parts of dioctyl phthalate, 5-6 parts of stearic acid, melamine tree
30-60 parts of fat.
The inventive concept total as one, another aspect of the present invention provide a kind of above-mentioned fire-retardant wood-fibred enhancing polyethylene
The manufacturing method of flexible web, includes the following steps：
(1), wood-fibred is bleached with degreasing bleaching liquid degreasing, wood-fibred, high polymerization degree APP after degreasing is bleached,
Precipitated calcium carbonate, silane coupling A -172, chlorinated paraffin, dioctyl phthalate and stearic acid mix in high speed mixing smelting machine
Refining is uniform, obtains premix；
(2), sprayed under high velocity agitation into step (1) described premix the melmac of atomization to premix into
Row cladding；
(3), the premix after coating melmac is dried, and then will be done in high low speed batch mixing blender
Premix after dry melmac cladding is kneaded uniformly with linear low density polyethylene resin, obtains mixture；
(4), step (3) described mixture is cooling fixed by kneading extrusion, mill tabletting, press polish overlay film, molding successively
Type and cutting deburring enhance polyethylene flexible web to get fire-retardant wood-fibred.
High polymerization degree APP, precipitated calcium carbonate, silane coupling A -172, chlorinated paraffin, neighbour are added into wood-fibred
Dioctyl phthalate and stearic acid are kneaded uniformly, are enhancing component with wood-fibred, high polymerization degree APP is fire retardant, chlorine
Fossil waxes are lubricant, and precipitated calcium carbonate is filler, and silane coupling A -172 is coupled, dioctyl phthalate conduct
Plasticizer, stearic acid coat above-mentioned raw materials as heat stabilizer, and using melmac, and it is multiple to form intumescent
Flame-retardant system is closed, the fire retardant performance of polyethylene flexible web is effectively improved, in the intumescent composite flame retardant system, wood
Fiber is charcoal source, high polymerization degree APP is acid source, melmac is air source, non-ignitable precipitated calcium carbonate and chlorination stone
Wax plays the role of cooperative flame retardant.Wherein, high polymerization degree APP is higher with decomposition temperature, hygroscopicity is smaller, processing performance
The advantages that preferable, is highly suitable to be applied for being used as fire-retardant host agent in flexible web.
The present invention is fine as basis material, the rational degreasing bleaching wood of Size Distribution using linear low density polyethylene resin
Dimension passes through melamine tree as filler as reinforcement, suitable precipitated calcium carbonate using the coupled action of silane coupling agent
Fat coats the mixture of above-mentioned substance, and combines raw material to be kneaded, mediates the collection of the technologies such as extrusion, mill tabletting in groups
It closes, substantially increases the mechanical strength of polyethylene flexible web.Wherein, linear low density polyethylene resin is ethylene and a small amount of height
The copolymer that is polymerized in the presence of a catalyst of grade alpha-olefin, has higher softening temperature and melting temperature, have intensity it is big,
The advantages that good toughness, big, heat-resisting, cold resistance is good rigidity, also has good environmental stress crack resistance, impact strength, resistance to
The performances such as tearing strength are conducive to the mechanical strength for improving flexible web using it as basis material.
Above-mentioned manufacturing method, it is preferred that in the step (1), degreasing bleaching liquid is prepared by the following method：It will
The disodium ethylene diamine tetraacetate and 0.1 parts by weight for the hydrogen peroxide, 0.05 parts by weight that the mass fraction of 12-15 parts by weight is 30%
Sodium pyrophosphate is added in the water of 80-100 parts by weight, adds the sodium hydroxide of 0.5-1.0 parts by weight, stirring and dissolving to get
Degreasing bleaching liquid.
Above-mentioned manufacturing method, it is preferred that in the step (1), the specific of wood-fibred is bleached with degreasing bleaching liquid degreasing
Process is：In bleaching case, according to 100：20 wood-fibred is sprayed with degreasing bleaching liquid weight ratio into the wood-fibred of high-speed stirred
Free and easy fat bleaching liquid, then insulation reaction 2-4h at a temperature of 50-60 DEG C.It is added to using the wood-fibred by degreasing bleaching poly-
The aesthetic quality of polyethylene coiled material can be improved in ethylene, the polyethylene coiled material of manufacture can need not pad pasting.
Above-mentioned manufacturing method, it is preferred that the preparation method of the melmac is as follows：It is 37% by mass fraction
100 parts by weight of formalin, 15 parts by weight of melamine and mass fraction be 30% 10 parts by weight of hydrogen peroxide mix, use
10% sodium hydrate aqueous solution adjusts mixed solution pH to 7-8, is heated to 65 DEG C of insulated and stirred 20min, is continuously heating to
90 DEG C are stirred to react 2h, are distilled to recover excessive formaldehyde and remove excessive water, mixed solution solid content is adjusted to 50-
60% to get melmac.
Above-mentioned manufacturing method, it is preferred that in the step (3), the premix after melmac is coated carries out
Drying specifically refers to：Premix after melmac is coated be put into microwave fiber powder drier dry to moisture content≤
8%, the wherein microwave frequency of microwave fiber powder drier is 2400-2500MHz, microwave power 1.5-2.5kW, transmission speed
For 0.4-0.6m/s.
Above-mentioned manufacturing method, it is preferred that in the step (4), mediate extrusion operation and specifically refer to：Mixture is put into
Kneading extrusion is carried out in twin-screw kneading extruder, the wherein die gap of twin-screw kneading extruder is 0.060~0.10in,
One section of temperature is 105-115 DEG C, and two sections of temperature are 115-155 DEG C, and outlet temperature is 155-175 DEG C, and machine neck die temperature is
155-175 DEG C, screw speed 10-25r/min, kneading finds time as 8-12min.
Above-mentioned manufacturing method, it is preferred that in the step (4), mill sheeting operation specifically refers to：To through kneading and squeeze
Material after going out is put into two roll tablet open mills progress mill tabletting, and wherein mixing temperature is 150-180 DEG C, when mill tabletting
Between be 12-18min.
Above-mentioned manufacturing method, it is preferred that in the step (4), the operation of press polish overlay film specifically refers to：Mill pressure will be passed through
Material after piece carries out press polish overlay film on three roller overlay film calenders, and wherein calendering temperature is 60-100 DEG C, and the press polish time is
2.5-3.5min；Molding cooling and shaping operation specifically refers to：Material after press polish overlay film is carried out in oil pressure cooling calibrator
Cooling and shaping, wherein cooling and shaping temperature are 30-50 DEG C, and the cooling and shaping time is 2.5-3.5min, and cooling and shaping thickness is 2-
5mm。
Above-mentioned manufacturing method, it is preferred that the Size Distribution of the wood-fibred is：The wood-fibred of 10-20 mesh accounts for wood-fibred
The wood-fibred of the 10-15% of total weight, 20-40 mesh accounts for the 50-60% of wood-fibred total weight, and the wood-fibred of 40-80 mesh accounts for the wooden fibre
The 10-15% of total weight is tieed up, the wood-fibred of 80-120 mesh accounts for the 5-10% of wood-fibred total weight, suitable wood fiber dimension distribution
Be conducive to the tensile strength for improving polyethylene coiled material, the flexibility for ensureing polyethylene coiled material；The linear low density polyethylene tree
Fat is milky white granules, density 0.916-0.921g/cm3, softening point is 110-125 DEG C, melt flow rate (MFR) 1.5-
2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, elongation at break >=500%, dart impact strength >=
80g；The high polymerization degree APP is white powder, wherein mass fraction >=71% of phosphorus pentoxide, nitrogen content >=
14%, the pH of average degree of polymerization >=1000,10g/L high polymerization degree APP solution is 4.5-6.5, decomposition temperature >=270
℃；Content >=98% of calcium carbonate, ferric oxide content≤0.20%, whiteness >=96%, pH are in the precipitated calcium carbonate
9-10, oil absorption >=50g/100g, salt acid-soluble substance≤0.5%, moisture≤0.8%；The matter of the chlorine in chlorinated paraffin
Amount score is 51-53%, refractive index 1.510-1.513.
Compared with the prior art, the advantages of the present invention are as follows：
(1) present invention using linear low density polyethylene (LLDPE) as base material, the wood-fibred after being bleached using degreasing as reinforcement, mainly with
High polymerization degree APP, melmac, precipitated calcium carbonate, wood-fibred and chlorinated paraffin are intumescent composite flame-proof body
It is that the polyethylene flexible web wood-fibred content manufactured is high, light-weight, mechanical strength is big, flexibility is good, fire-retardant fireproof,
It can be used as airport, station, hotel, the flexible floor file floor in room and flexible decorating material.
(2) present invention initiates the melmac that atomization is sprayed into material mixing process, with to wood-fibred, high polymerization
Degree ammonium polyphosphate and precipitated calcium carbonate etc. are coated, and intumescent composite flame-retardant agent are obtained, and in existing fire retardant coating technology
The operating processes such as cumbersome solvent suspension, dispersion, package, drying are compared, and fire retardant preparation method step of the invention is simpler
List, operation are more convenient；Also, the intumescent composite flame-retardant agent coated using this method is added in polyethylene, it can
Efficiently solve the problem of declining due to the incompatible caused wood plastic composite mechanical strength in interface.
(3) microwave drying process is used once to remove the water in raw material, degreasing bleaching wood-fibred and melmac
Point, it effectively simplifies operating process, reduce energy consumption.
(4) pass through the association of high polymerization degree APP, wood-fibred, chlorinated paraffin, precipitated calcium carbonate and melmac
Same-action and high polymerization degree APP, wood-fibred, chlorinated paraffin, precipitated calcium carbonate and melmac are using specific
Composition and ratio so that polyethylene flexible web of the invention has good fire-retardant fireproof characteristic.
(5) wood-fibred, suitable lightweight carbon are bleached by type low density polyethylene resin, the rational degreasing of Size Distribution
Sour calcium, the coupled action of silane coupling agent, melmac cladding, raw material are kneaded the integrated combination for mediating the technologies such as mill,
So that the polyethylene flexible web of the present invention has good strength characteristics.
(6) type low density polyethylene resin is used to be utilized using the rational wood-fibred of Size Distribution as basis material
The coupled action of silane coupling agent, chlorinated paraffin-dioctyl phthalate of optimization-stearic acid proportioning, melmac
The integrated combination of the technologies such as cladding so that the polyethylene flexible web has good flexibility.
Specific implementation mode
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
A kind of embodiment of the fire-retardant wood-fibred enhancing polyethylene flexible web of the present invention and its manufacturing method, the fire-retardant wood are fine
Dimension enhancing polyethylene flexible web includes the component of following parts by weight：Linear low density polyethylene resin 55kg, wood-fibred 50kg,
High polymerization degree APP 9kg, precipitated calcium carbonate 90kg, -172 2.5kg of silane coupling A, chlorinated paraffin 11kg, adjacent benzene two
Formic acid dioctyl ester 5kg, stearic acid 5kg, melmac 50kg.Wherein, linear low density polyethylene resin is nontoxic, nothing
Taste, odorless milky white granules, density is in 0.916-0.921g/cm3In range, softening point is 110-125 DEG C, melt flows speed
Rate 1.5-2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, elongation at break >=500%, dart impact are strong
Degree >=80g；The Size Distribution of wood-fibred is：10-20 purposes account for the 10-15% of wood-fibred total weight, and 20-40 purposes account for wood-fibred
The 50-60% of total weight, 40-80 purpose account for the 10-15% of wood-fibred total weight, and 80-120 purposes account for the 5- of wood-fibred total weight
10%；High polymerization degree APP is white powder, phosphorus pentoxide (P2O5) mass fraction >=71%, nitrogen content >=
14%, average degree of polymerization >=1000, pH value (10g/L solution) is 4.5-6.5 ,/w% >=99 granularity (45 μm of ＜), solubility (g/
100ml water, 25 DEG C)≤0.5, decomposition temperature >=270 DEG C；Calcium carbonate content >=98% in precipitated calcium carbonate, di-iron trioxide contain
Amount≤0.20%, whiteness >=96%, pH value 9-10, oil absorption >=50g/100g, salt acid-soluble substance≤0.5%, moisture content≤
0.8%；The mass fraction of chlorine in chlorinated paraffin be 51-53%, thermal stability factor (175 DEG C, 4h, nitrogen 10L/h) (HCl)≤
0.10%, heating loss (130 DEG C, 2h)≤0.3%, coloration (platinum-brill color number)≤100, density (p50)/(g/cm3) be
1.23-1.25, viscosity (50 DEG C)/mPaS150-250≤300, refractive index 1.510-1.513.
The manufacturing method of the fire-retardant wood-fibred enhancing polyethylene flexible web includes the following steps：
It (1), (should to the 50kg wood-fibreds sprinkling 10kg degreasings bleaching liquid under high-speed stirred with spraying machine in bleaching case
The disodium ethylene diamine tetraacetate of hydrogen peroxide, 0.05 parts by weight that degreasing bleaching liquid is 30% by the mass fraction of 12-15 parts by weight
It is added to the sodium pyrophosphate of 0.1 parts by weight in the water of 80-100 parts by weight, adds the sodium hydroxide of 0.5-1.0 parts by weight,
Stirring and dissolving obtains.), it then seals, insulation reaction 3h at a temperature of 50 DEG C, then wood-fibred, 9kg after degreasing is bleached
High polymerization degree APP (APP), 90kg precipitated calcium carbonates, 2.5kg silane coupling As -172,11kg chlorinated paraffins, 5kg are adjacent
Dioctyl phthalate and 5kg stearic acid are kneaded uniformly in high speed mixing smelting machine, obtain premix.
(2), the melamine tree of atomization is sprayed into glue sprayer into premix obtained by step (1) in the case where high speed is kneaded stirring
Fat 50kg coats premix, wherein melmac is prepared by the following method：It is 37% by mass fraction
10 parts by weight of hydrogen peroxide that 100 parts by weight of formalin, 15 parts by weight of melamine and mass fraction are 30% mix, with 10%
Sodium hydrate aqueous solution adjusts mixed solution pH to 7, is heated to 65 DEG C of insulated and stirred 20min, is continuously heating to 90 DEG C and stirs
Reaction 2h is mixed, excessive formaldehyde is distilled to recover and removes excessive water, mixed solution solid content is adjusted to 50%.
(3), the premix after melmac coats is put into microwave fiber powder drier and is dried to aqueous
Rate is 8%, and wherein the microwave frequency of microwave fiber powder drier is 2400-2500MHz, microwave power 1.5-2.5kW, transmission
Speed is 0.5m/s；Then the premix after coating dry melmac in high low speed batch mixing blender and 55kg
Linear low density polyethylene resin is kneaded uniformly, obtains mixture.
(4), mixture obtained by step (3) is put into twin-screw kneading extruder and carries out kneading extrusion, wherein twin-screw
The die gap of kneading extruder is 0.060-0.10in, and one section of temperature is 110 DEG C, and two sections of temperature are 120 DEG C, and outlet temperature is
160 DEG C, machine neck die temperature is 160 DEG C, screw speed 10-25r/min, and kneading finds time as 10min.Then it will mediate
Material after extrusion is put into two roll tablet open mills progress mill tabletting, wherein mixing temperature is 150 DEG C, when mill tabletting
Between be 15min.Material after mill tabletting is carried out to press polish overlay film on three roller overlay film calenders again, wherein press polish temperature
Degree is 80 DEG C, and the press polish time is 3min.Institute's coating layer includes, under the melamine dipping decorative paper with decorative pattern is constituted
Superficial film, the upper table face mask layer being made of melamine-impregnated alundum (Al2O3) abrasion-proof paper and the bottom surface being made of non-woven fabrics
Layer.Material after press polish overlay film is subjected to cooling and shaping in oil pressure cooling calibrator, wherein cooling and shaping temperature is 30 DEG C,
The cooling and shaping time is 3min, and cooling and shaping thickness is 2-5mm；Finally by the material after cooling and shaping in dragger, cutting machine
With carry out cutting deburring under the action of trimmer, baling press packaging to get to fire-retardant wood-fibred enhancing polyethylene flexible web at
The thickness of product, the fire-retardant wood-fibred enhancing polyethylene flexible web is 2-5mm, width 2440mm, length 50m.
The combustibility of polyethylene flexible web is enhanced to the fire-retardant wood-fibred and mechanical property is tested, test result
As shown in table 1.
Embodiment 2
A kind of embodiment of the fire-retardant wood-fibred enhancing polyethylene flexible web of the present invention and its manufacturing method, the fire-retardant wood are fine
Dimension enhancing polyethylene flexible web includes the component of following parts by weight：Linear low density polyethylene resin 60kg, wood-fibred 40kg,
High polymerization degree APP 8kg, precipitated calcium carbonate 90kg, -172 2.5kg of silane coupling A, chlorinated paraffin 11kg, adjacent benzene two
Formic acid dioctyl ester 5kg, stearic acid 5kg, melmac 50kg.Wherein, linear low density polyethylene resin is nontoxic, nothing
Taste, odorless milky white granules, density is in 0.916-0.921g/cm3In range, softening point is 110-125 DEG C, melt flows speed
Rate 1.5-2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, elongation at break >=500%, dart impact are strong
Degree >=80g；The Size Distribution of wood-fibred is：10-20 purposes account for the 10-15% of wood-fibred total weight, and 20-40 purposes account for wood-fibred
The 50-60% of total weight, 40-80 purpose account for the 10-15% of wood-fibred total weight, and 80-120 purposes account for the 5- of wood-fibred total weight
10%；High polymerization degree APP is white powder, phosphorus pentoxide (P2O5) mass fraction >=71%, nitrogen content >=
14%, average degree of polymerization >=1000, pH value (10g/L solution) is 4.5-6.5 ,/w% >=99 granularity (45 μm of ＜), solubility (g/
100ml water, 25 DEG C)≤0.5, decomposition temperature >=270 DEG C；Calcium carbonate content >=98% in precipitated calcium carbonate, di-iron trioxide contain
Amount≤0.20%, whiteness >=96%, pH value 9-10, oil absorption >=50g/100g, salt acid-soluble substance≤0.5%, moisture content≤
0.8%；The mass fraction of chlorine in chlorinated paraffin be 51-53%, thermal stability factor (175 DEG C, 4h, nitrogen 10L/h) (HCl)≤
0.10%, heating loss (130 DEG C, 2h)≤0.3%, coloration (platinum-brill color number)≤100, density (p50)/(g/cm3) be
1.23-1.25, viscosity (50 DEG C)/mPaS150-250≤300, refractive index 1.510-1.513.
The manufacturing method of the fire-retardant wood-fibred enhancing polyethylene flexible web includes the following steps：
(1), in bleaching case, with spraying machine, to the 40kg wood-fibreds sprinkling 8kg degreasings bleaching liquid under high-speed stirred, (this is de-
Fat bleaching liquid by 12-15 parts by weight mass fraction be 30% hydrogen peroxide, 0.05 parts by weight disodium ethylene diamine tetraacetate and
The sodium pyrophosphate of 0.1 parts by weight is added in the water of 80-100 parts by weight, is added the sodium hydroxide of 0.5-1.0 parts by weight, is stirred
Dissolving is mixed to obtain.), it then seals, insulation reaction 4h at a temperature of 55 DEG C, then wood-fibred, 8kg high after degreasing is bleached
Degree of polymerization ammonium polyphosphate, 90kg precipitated calcium carbonates, 2.5kg silane coupling As -172,11kg chlorinated paraffins, 5kg phthalic acids
Dioctyl ester and 5kg stearic acid are kneaded uniformly in high speed mixing smelting machine, obtain premix.
(2), the melamine tree of atomization is sprayed into glue sprayer into premix obtained by step (1) in the case where high speed is kneaded stirring
Fat 50kg coats premix, wherein melmac is prepared by the following method：It is 37% by mass fraction
10 parts by weight of hydrogen peroxide that 100 parts by weight of formalin, 15 parts by weight of melamine and mass fraction are 30% mix, with 10%
Sodium hydrate aqueous solution adjusts mixed solution pH to 7-8, is heated to 65 DEG C of insulated and stirred 20min, is continuously heating to 90 DEG C
It is stirred to react 2h, be distilled to recover excessive formaldehyde and removes excessive water, mixed solution solid content is adjusted to 55%.
(3), the premix after melmac coats is put into microwave fiber powder drier and is dried to aqueous
Rate is 6%, and wherein the microwave frequency of microwave fiber powder drier is 2400-2500MHz, microwave power 1.5-2.5kW, transmission
Speed is 0.5m/s；Then the premix after coating dry melmac in high low speed batch mixing blender and 60kg
Linear low density polyethylene resin is kneaded uniformly, obtains mixture.
(4), mixture obtained by step (3) is put into twin-screw kneading extruder and carries out kneading extrusion, wherein twin-screw
The die gap of kneading extruder is 0.060-0.10in, and one section of temperature is 110 DEG C, and two sections of temperature are 120 DEG C, and outlet temperature is
155 DEG C, machine neck die temperature is 155 DEG C, screw speed 10-25r/min, and kneading finds time as 10min.Then it will mediate
Material after extrusion is put into two roll tablet open mills progress mill tabletting, wherein mixing temperature is 150 DEG C, when mill tabletting
Between be 15min.Material after mill tabletting is carried out to press polish overlay film on three roller overlay film calenders again, wherein press polish temperature
Degree is 80 DEG C, and the press polish time is 3min.Institute's coating layer includes, under the melamine dipping decorative paper with decorative pattern is constituted
Superficial film, the upper table face mask layer being made of melamine-impregnated alundum (Al2O3) abrasion-proof paper and the bottom surface being made of non-woven fabrics
Layer.Material after press polish overlay film is subjected to cooling and shaping in oil pressure cooling calibrator, wherein cooling and shaping temperature is 30 DEG C,
The cooling and shaping time is 3min, and cooling and shaping thickness is 2-5mm；Finally by the material after cooling and shaping in dragger, cutting machine
With carry out cutting deburring under the action of trimmer, baling press packaging to get to fire-retardant wood-fibred enhancing polyethylene flexible web at
The thickness of product, the fire-retardant wood-fibred enhancing polyethylene flexible web is 2-5mm, width 2440mm, length 50m.
The combustibility of polyethylene flexible web is enhanced to the fire-retardant wood-fibred and mechanical property is tested, test result
As shown in table 1.
Embodiment 3
A kind of embodiment of the fire-retardant wood-fibred enhancing polyethylene flexible web of the present invention and its manufacturing method, the fire-retardant wood are fine
Dimension enhancing polyethylene flexible web includes the component of following parts by weight：The wood of linear low density polyethylene resin 60kg, 60-80 mesh
Fiber 40kg, high polymerization degree APP 8kg, precipitated calcium carbonate 90kg, -172 2.5kg of silane coupling A, chlorinated paraffin
11kg, dioctyl phthalate 5kg, stearic acid 5kg, melmac 50kg.Wherein, linear low density polyethylene resin
For nontoxic, tasteless, odorless milky white granules, density is in 0.916-0.921g/cm3In range, softening point is 110-125 DEG C,
Melt flow rate (MFR) 1.5-2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, elongation at break >=500%,
Dart impact strength >=80g；High polymerization degree APP is white powder, the mass fraction of phosphorus pentoxide (P2O5) >=
71%, nitrogen content >=14%, average degree of polymerization >=1000, pH value (10g/L solution) is 4.5-6.5, granularity (45 μm of ＜)/w%
>=99, solubility (g/100ml water, 25 DEG C)≤0.5, decomposition temperature >=270 DEG C；Calcium carbonate content in precipitated calcium carbonate >=
98%, ferric oxide content≤0.20%, whiteness >=96%, pH value 9-10, oil absorption >=50g/100g, salt acid-soluble substance
≤ 0.5%, moisture content≤0.8%；The mass fraction of chlorine in chlorinated paraffin be 51-53%, thermal stability factor (175 DEG C, 4h, nitrogen
10L/h) (HCl)≤0.10%, heating loss (130 DEG C, 2h)≤0.3%, coloration (platinum-brill color number)≤100, density (p50)/
(g/cm3) it is 1.23-1.25, viscosity (50 DEG C)/150-250≤300 mPaS, refractive index 1.510-1.513.
The manufacturing method of the fire-retardant wood-fibred enhancing polyethylene flexible web includes the following steps：
(1), in bleaching case, 8kg degreasings are sprayed to the wood-fibred of the 40kg 60-80 mesh under high-speed stirred with spraying machine
Bleaching liquid (the ethylenediamine tetraacetic of hydrogen peroxide, 0.05 parts by weight that the degreasing bleaching liquid is 30% by the mass fraction of 12-15 parts by weight
Acetic acid disodium and the sodium pyrophosphate of 0.1 parts by weight are added in the water of 80-100 parts by weight, add the hydrogen of 0.5-1.0 parts by weight
Sodium oxide molybdena, stirring and dissolving obtain.), it then seals, insulation reaction 2h at a temperature of 60 DEG C, then the wood after degreasing is bleached
Fiber, 8kg high polymerization degree APPs, 90kg precipitated calcium carbonates, 2.5kg silane coupling As -172,11kg chlorinated paraffins, 5kg
Dioctyl phthalate and 5kg stearic acid are kneaded uniformly in high speed mixing smelting machine, obtain premix.
(2), the melamine tree of atomization is sprayed into glue sprayer into premix obtained by step (1) in the case where high speed is kneaded stirring
Fat 50kg coats premix, wherein melmac is prepared by the following method：It is 37% by mass fraction
10 parts by weight of hydrogen peroxide that 100 parts by weight of formalin, 15 parts by weight of melamine and mass fraction are 30% mix, with 10%
Sodium hydrate aqueous solution adjusts mixed solution pH to 7-8, is heated to 65 DEG C of insulated and stirred 20min, is continuously heating to 90 DEG C
It is stirred to react 2h, be distilled to recover excessive formaldehyde and removes excessive water, mixed solution solid content is adjusted to 60%.
(3), the premix after melmac coats is put into microwave fiber powder drier and is dried to aqueous
Rate is 8%, and wherein the microwave frequency of microwave fiber powder drier is 2400-2500MHz, microwave power 1.5-2.5kW, transmission
Speed is 0.5m/s；Then the premix after coating dry melmac in high low speed batch mixing blender and 60kg
Linear low density polyethylene resin is kneaded uniformly, obtains mixture.
(4), mixture obtained by step (3) is put into twin-screw kneading extruder and carries out kneading extrusion, wherein twin-screw
The die gap of kneading extruder is 0.060-0.10in, and one section of temperature is 110 DEG C, and two sections of temperature are 120 DEG C, and outlet temperature is
155 DEG C, machine neck die temperature is 155 DEG C, screw speed 10-25r/min, and kneading finds time as 10min.Then it will mediate
Material after extrusion is put into two roll tablet open mills progress mill tabletting, wherein mixing temperature is 150 DEG C, when mill tabletting
Between be 15min.Material after mill tabletting is carried out to press polish overlay film on three roller overlay film calenders again, wherein press polish temperature
Degree is 80 DEG C, and the press polish time is 3min.Institute's coating layer includes, under the melamine dipping decorative paper with decorative pattern is constituted
Superficial film, the upper table face mask layer being made of melamine-impregnated alundum (Al2O3) abrasion-proof paper and the bottom surface being made of non-woven fabrics
Layer.Material after press polish overlay film is subjected to cooling and shaping in oil pressure cooling calibrator, wherein cooling and shaping temperature is 30 DEG C,
The cooling and shaping time is 3min, and cooling and shaping thickness is 2-5mm；Finally by the material after cooling and shaping in dragger, cutting machine
With carry out cutting deburring under the action of trimmer, baling press packaging to get to fire-retardant wood-fibred enhancing polyethylene flexible web at
The thickness of product, the fire-retardant wood-fibred enhancing polyethylene flexible web is 2-5mm, width 2440mm, length 50m.
The combustibility of polyethylene flexible web is enhanced to the fire-retardant wood-fibred and mechanical property is tested, test result
As shown in table 1.
Comparative example 1
A kind of embodiment of the fire-retardant wood-fibred enhancing polyethylene flexible web of the present invention and its manufacturing method, the fire-retardant wood are fine
Dimension enhancing polyethylene flexible web includes the component of following parts by weight：Linear low density polyethylene resin 80kg, wood-fibred 20kg,
High polymerization degree APP 3kg, precipitated calcium carbonate 90kg, -172 2.5kg of silane coupling A, chlorinated paraffin 11kg, adjacent benzene two
Formic acid dioctyl ester 5kg, stearic acid 5kg, melmac 0kg.Wherein, linear low density polyethylene resin be it is nontoxic, tasteless,
Odorless milky white granules, density is in 0.916-0.921g/cm3In range, softening point is 110-125 DEG C, melt flow rate (MFR)
1.5-2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, elongation at break >=500%, dart impact strength
≥80g；The Size Distribution of wood-fibred is：10-20 purposes account for the 10-15% of wood-fibred total weight, and it is total that 20-40 purposes account for wood-fibred
The 50-60% of weight, 40-80 purpose account for the 10-15% of wood-fibred total weight, and 80-120 purposes account for the 5- of wood-fibred total weight
10%；High polymerization degree APP is white powder, phosphorus pentoxide (P2O5) mass fraction >=71%, nitrogen content >=
14%, average degree of polymerization >=1000, pH value (10g/L solution) is 4.5-6.5 ,/w% >=99 granularity (45 μm of ＜), solubility (g/
100ml water, 25 DEG C)≤0.5, decomposition temperature >=270 DEG C；Calcium carbonate content >=98% in precipitated calcium carbonate, di-iron trioxide contain
Amount≤0.20%, whiteness >=96%, pH value 9-10, oil absorption >=50g/100g, salt acid-soluble substance≤0.5%, moisture content≤
0.8%；The mass fraction of chlorine in chlorinated paraffin be 51-53%, thermal stability factor (175 DEG C, 4h, nitrogen 10L/h) (HCl)≤
0.10%, heating loss (130 DEG C, 2h)≤0.3%, coloration (platinum-brill color number)≤100, density (p50)/(g/cm3) be
1.23-1.25, viscosity (50 DEG C)/mPaS150-250≤300, refractive index 1.510-1.513.
The manufacturing method of the fire-retardant wood-fibred enhancing polyethylene flexible web includes the following steps：
(1), in bleaching case, with spraying machine, to the 20kg wood-fibreds sprinkling 4kg degreasings bleaching liquid under high-speed stirred, (this is de-
Fat bleaching liquid by 12-15 parts by weight mass fraction be 30% hydrogen peroxide, 0.05 parts by weight disodium ethylene diamine tetraacetate and
The sodium pyrophosphate of 0.1 parts by weight is added in the water of 80-100 parts by weight, is added the sodium hydroxide of 0.5-1.0 parts by weight, is stirred
Dissolving is mixed to obtain.), it then seals, insulation reaction 3h at a temperature of 55 DEG C, then wood-fibred, 3kg high after degreasing is bleached
Degree of polymerization ammonium polyphosphate, 90kg precipitated calcium carbonates, 2.5kg silane coupling As -172,11kg chlorinated paraffins, 5kg phthalic acids
Dioctyl ester and 5kg stearic acid are kneaded uniformly in high speed mixing smelting machine, obtain premix.
(2), it is 8%, wherein microwave fiber dried bean noodles premix to be put into drying to moisture content in microwave fiber powder drier
The microwave frequency of dry machine is 2400-2500MHz, microwave power 1.5-2.5kW, transmission speed 0.5m/s；Then in height
Dry premix and 80kg linear low density polyethylene resins are kneaded uniformly in fast batch mixing blender, obtain mixture.
(3), mixture obtained by step (2) is put into twin-screw kneading extruder and carries out kneading extrusion, wherein twin-screw
The die gap of kneading extruder is 0.060-0.10in, and one section of temperature is 90 DEG C, and two sections of temperature are 100 DEG C, and outlet temperature is
140 DEG C, machine neck die temperature is 140 DEG C, screw speed 10-25r/min, and kneading finds time as 10min.Then it will mediate
Material after extrusion is put into two roll tablet open mills progress mill tabletting, wherein mixing temperature is 120 DEG C, when mill tabletting
Between be 15min.Material after mill tabletting is carried out to press polish overlay film on three roller overlay film calenders again, wherein press polish temperature
Degree is 80 DEG C, and the press polish time is 3min.Institute's coating layer includes, under the melamine dipping decorative paper with decorative pattern is constituted
Superficial film, the upper table face mask layer being made of melamine-impregnated alundum (Al2O3) abrasion-proof paper and the bottom surface being made of non-woven fabrics
Layer.Material after press polish overlay film is subjected to cooling and shaping in oil pressure cooling calibrator, wherein cooling and shaping temperature is 30 DEG C,
The cooling and shaping time is 3min, and cooling and shaping thickness is 2-5mm；Finally by the material after cooling and shaping in dragger, cutting machine
With carry out cutting deburring under the action of trimmer, baling press packaging to get to fire-retardant wood-fibred enhancing polyethylene flexible web at
The thickness of product, the fire-retardant wood-fibred enhancing polyethylene flexible web is 2-5mm, width 2440mm, length 50m.
The combustibility and mechanical property of the flexible web are tested, test result is as shown in table 1.
The combustibility and mechanical performance data of 1 polyethylene flexible web of table compare
By table 1 as it can be seen that the fire-retardant wood-fibred enhancing polyethylene that the manufacturing method using the present invention of embodiment 1,2 and 3 obtains
Characteristic combustion parameter PHRR, mHRR and TSP of flexible web, which are significantly lower than in comparative example 1, does not use melmac to coat
The polyethylene flexible web and polyethylene that premix obtains, illustrate by wood-fibred, high polymerization degree APP, chlorinated paraffin and
Precipitated calcium carbonate etc. is mixed to form premix, and using melmac premix is coated can greatly improve it is poly-
The combustibility of ethylene flexible web.The stretching of embodiment 1,2 and 3 obtained flame-retardant wood-fibreds enhancing polyethylene flexible web is strong
Degree, impact strength, elongation at break and right angle tearing toughness are above comparative example 1, illustrate through melmac to pre-
Batch mixing, which carries out cladding, can improve the mechanical property of polyethylene flexible web.In addition, comparative example 2 and embodiment 3 are visible (real
Apply wood fiber dimension in example 2 to be reasonably distributed, wood-fibred is 60-80 mesh in embodiment 3), using the rational wood-fibred of Size Distribution
Be conducive to improve the combustibility and mechanical property of polyethylene flexible web.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of fire-retardant wood-fibred enhances polyethylene flexible web, which is characterized in that include the component of following parts by weight：It is linear low
50-60 parts of Density Polyethylene Resin, 40-60 parts of wood-fibred, 8-10 parts of high polymerization degree APP, precipitated calcium carbonate 80-100
Part, -172 2-3 parts of silane coupling A, 10-12 parts of chlorinated paraffin, 5-26 parts of dioctyl phthalate, 5-6 parts of stearic acid,
30-60 parts of melmac.
2. a kind of manufacturing method of fire-retardant wood-fibred enhancing polyethylene flexible web as described in claim 1, including following step
Suddenly：
(1), wood-fibred, wood-fibred, high polymerization degree APP after degreasing is bleached, lightweight are bleached with degreasing bleaching liquid degreasing
Calcium carbonate, silane coupling A -172, chlorinated paraffin, dioctyl phthalate and stearic acid are kneaded in high speed mixing smelting machine
It is even, obtain premix；
(2), the melmac for spraying into atomization into step (1) described premix under high velocity agitation wraps premix
It covers；
(3), the premix after coating melmac is dried, then will be dry in high low speed batch mixing blender
Premix after melmac cladding is kneaded uniformly with linear low density polyethylene resin, obtains mixture；
(4), by step (3) described mixture successively through kneading extrusions, mill tabletting, press polish overlay film, be molded cooling and shaping and
Cut deburring enhances polyethylene flexible web to get fire-retardant wood-fibred.
3. manufacturing method according to claim 2, which is characterized in that in the step (1), degreasing bleaching liquid is by such as lower section
Method is prepared：By the mass fraction of 12-15 parts by weight be 30% hydrogen peroxide, 0.05 parts by weight disodium ethylene diamine tetraacetate
It is added to the sodium pyrophosphate of 0.1 parts by weight in the water of 80-100 parts by weight, adds the sodium hydroxide of 0.5-1.0 parts by weight,
Stirring and dissolving is to get degreasing bleaching liquid.
4. manufacturing method according to claim 2, which is characterized in that in the step (1), wood is bleached with degreasing bleaching liquid
The detailed process of fiber is：In bleaching case, according to 100：20 wood-fibred and degreasing bleaching liquid weight ratio are to high-speed stirred
Degreasing bleaching liquid is sprayed in wood-fibred, then insulation reaction 2-4h at a temperature of 50-60 DEG C.
5. manufacturing method according to claim 2, which is characterized in that the preparation method of the melmac is as follows：
The hydrogen peroxide for being 30% by 100 parts by weight of formalin, 15 parts by weight of melamine and mass fraction that mass fraction is 37%
10 parts by weight mix, and adjust mixed solution pH to 7-8 with 10% sodium hydrate aqueous solution, are heated to 65 DEG C of insulated and stirreds
20min is continuously heating to 90 DEG C and is stirred to react 2h, is distilled to recover excessive formaldehyde and removes excessive water, mixed solution is consolidated
Content is adjusted to 50-60% to get melmac.
6. manufacturing method according to claim 2, which is characterized in that in the step (3), melmac is coated
Premix afterwards, which is dried, to be specifically referred to：Premix after melmac is coated is put into microwave fiber powder drier
Drying to moisture content≤8%, the wherein microwave frequency of microwave fiber powder drier is 2400-2500MHz, microwave power 1.5-
2.5kW, transmission speed 0.4-0.6m/s.
7. manufacturing method according to claim 2, which is characterized in that in the step (4), mediating extrusion operation is specifically
Refer to：Mixture is put into twin-screw kneading extruder and carries out kneading extrusion, wherein the die gap of twin-screw kneading extruder
For 0.060~0.10in, one section of temperature is 105-115 DEG C, and two sections of temperature are 115-155 DEG C, and outlet temperature is 155-175 DEG C,
Machine neck die temperature is 155-175 DEG C, screw speed 10-25r/min, and kneading finds time as 8-12min.
8. manufacturing method according to claim 2, which is characterized in that in the step (4), mill sheeting operation is specifically
Refer to：Kneading material after extrusion will be passed through and be put into progress mill tabletting in two roll tablet open mills, wherein mixing temperature is 150-
180 DEG C, the mill tabletting time is 12-18min.
9. manufacturing method according to claim 2, which is characterized in that in the step (4), the operation of press polish overlay film is specifically
Refer to：Material after mill tabletting is subjected to press polish overlay film on three roller overlay film calenders, wherein calendering temperature is 60-100
DEG C, the press polish time is 2.5-3.5min；Molding cooling and shaping operation specifically refers to：Material after press polish overlay film is cooled down in oil pressure
Cooling and shaping is carried out in forming machine, wherein cooling and shaping temperature is 30-50 DEG C, and the cooling and shaping time is 2.5-3.5min, cooling
Sizing thickness is 2-5mm.
10. according to the manufacturing method described in any one of claim 2-9, which is characterized in that the Size Distribution of the wood-fibred
For：The wood-fibred of 10-20 mesh accounts for the 10-15% of wood-fibred total weight, and the wood-fibred of 20-40 mesh accounts for the 50- of wood-fibred total weight
The wood-fibred of 60%, 40-80 mesh accounts for the 10-15% of wood-fibred total weight, and the wood-fibred of 80-120 mesh accounts for wood-fibred total weight
5-10%；The linear low density polyethylene resin is milky white granules, density 0.916-0.921g/cm3, softening point is
110-125 DEG C, melt flow rate (MFR) 1.5-2.5g/10min, mist degree≤14%, yield tensile strength >=8.3MPa, fracture stretches
Long rate >=500%, dart impact strength >=80g；The high polymerization degree APP is white powder, wherein phosphorus pentoxide
Mass fraction >=71%, nitrogen content >=14%, the pH of average degree of polymerization >=1000,10g/L high polymerization degree APP solution
For 4.5-6.5, decomposition temperature >=270 DEG C；Content >=98% of calcium carbonate in the precipitated calcium carbonate, ferric oxide content≤
0.20%, whiteness >=96%, pH 9-10, oil absorption >=50g/100g, salt acid-soluble substance≤0.5%, moisture≤
0.8%；The mass fraction of the chlorine in chlorinated paraffin is 51-53%, refractive index 1.510-1.513.
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