CN103613834B - A kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method - Google Patents

A kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method Download PDF

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CN103613834B
CN103613834B CN201310579753.8A CN201310579753A CN103613834B CN 103613834 B CN103613834 B CN 103613834B CN 201310579753 A CN201310579753 A CN 201310579753A CN 103613834 B CN103613834 B CN 103613834B
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foam material
rubber
smoke
flame retardant
modified poly
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CN103613834A (en
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李崇
李士学
王永明
高之香
李建武
吴子刚
张卫军
唐斌
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Sanyou Tianjin Macromolecular Techonoloy Co Ltd
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Sanyou Tianjin Macromolecular Techonoloy Co Ltd
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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
    • 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
    • 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
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7404—Mixing devices specially adapted for foamable substances
    • B29B7/7409—Mixing devices specially adapted for foamable substances with supply of gas
    • B29B7/7428—Methodical aspects
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102—Azo-compounds
    • C08J9/103—Azodicarbonamide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
    • C08J9/105—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/14—Applications used for foams
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention provides a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method.Present method first prepares foaming concentrate with plastic banbury mixer: linear low density polyethylene resin and nucleator are dropped into Banbury mixer, then adds second Warburg Pincus rubber and the banburying of olefin type elastomer resin; Again terpolymer EP rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer banburying, last discharge is foaming concentrate; Then foamed material mixture is prepared with mill: foaming concentrate is entered mill with whipping agent, frothing aid, linking agent, crosslinking coagent and mixes; Foamed material mixture is sent into the sheet material of extruder for shaping, be automobile cavity low-smoke and flame retardant modified poly ethylene foam material.This foam material is when 140-180 DEG C, and height multiplying power >=800%, expansion ratio is more than 3000%.Thus reaching the low cigarette, fire-retardant of expection, foaming rear surface is soft and without hard excellent effect of separating, and improves environmental protection and the security of automobile.

Description

A kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method
Technical field
The present invention relates to the preparation of foam material, particularly relate to a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method.
Background technology
Flourish along with Car Industry, people are not only interested in the visual experience intuitively such as profile, color of automobile, and the comfortableness to bring to us automobile and security are also paid much attention to, and the key point weighing comfort level is exactly automobile vibrations produced in the process of moving and noise, so the cavity resonance that minimizing automobile produces under steam, the noise pollution that reduction automobile cavity inside produces due to air circulation and vibrations friction is extremely important.And the flame retardant resistance of automobile material therefor also must be paid attention to.
Current automobile cavity foam material generally takes EVA to be material of main part, first EVA material does not have flame retardant effect, meets fiery easy firing, and secondly the maximum expansion ratio of EVA material is generally at about 25 times, and height multiplying power is generally at about 5 times, limited to the complete fillibility contribution of automobile cavity.
Summary of the invention
In view of above-mentioned prior art Problems existing and defect, the invention provides a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method.The material adopting present method to prepare is mainly used in automobile A, B, C, D post and the filling of the large cavity of wheel cover of automobile, fully blocks wind and makes an uproar by the transmission of large cavity, reduces decibel under steam in car.
The material of main part that the present invention adopts is linear low density polyethylene resin, and main manifestations is that foam volume is large, can play the effect of the density after reducing material volume and product foaming.But easily produce cracking due to material after foaming and firmly to separate, easily come off in the cavities, and product is inflammable, linear low density polyethylene resin can not address these problems well, also contributes deficiency to realization height multiplying power simultaneously.So add terpolymer EP rubber and cis-1,4-polybutadiene rubber in linear low density polyethylene resin, soft after playing product foaming, effect not easy to crack.And add second Warburg Pincus rubber and mainly play two effects: 1. second Warburg Pincus rubber has good flame retardant resistance, can serve as the effect of fire retardant in formula for a product; 2. second Warburg Pincus rubber possesses again the characteristic of ethylene-vinyl acetate copolymer, and during high temperature, surface has initial bonding strength, can paste with panel beating well.Adding olefin type elastomer resin plays a part larger for the height multiplying power after the foaming of raising product.
The technical scheme that the present invention takes is: a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method, and it is characterized in that, the method is carried out according to following steps:
Step one: plastic banbury mixer prepares foaming concentrate
Linear low density polyethylene resin, second Warburg Pincus rubber, terpolymer EP rubber, olefin type elastomer resin, cis-1,4-polybutadiene rubber and nucleator are fed intake in order: first linear low density polyethylene resin is dropped into Banbury mixer, then nucleator is added, when banburying temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin, the banburying time is 4-8 minute, be vented 2-5 time, again terpolymer EP rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer, the banburying time is 2-5 minute, last discharge, is foaming concentrate.
Step 2: foamed material mixture is prepared in mill
The foaming concentrate prepared through step one and whipping agent, frothing aid, linking agent, crosslinking coagent are entered mill mixing 10-20 minute, and mixing temperature controls at 80-100 DEG C;
Step 3: the foamed material mixture prepared through step 2 is sent into forcing machine, and the sheet material of extrusion moulding under extruder temperature is 80-100 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Feature of the present invention is, the plastic foamed goods that the foam material adopting present method to prepare is processed are little due to its density, achieve car light; This foaming materials volume is large, can save material cost; Foaming product good with type, is easy to constructing operation; This material has the large feature of unidirectional expansion ratio, and height multiplying power >=800%, is conducive to filling large cavity.This is one of maximum feature of the present invention.
The low cigarette that this foam material realizes, fire-retardant feature are different from other foamed products and add fire retardant, but the anti-flaming function had by second Warburg Pincus rubber components self realization, therefore improve environmental protection and the security of automobile.Thus reach the filling meeting the large cavity of automobile, intercept the circulation of automobile cavity air, to the object of Integral automobile damping noise reduction.This material has good market outlook in the application of the large cavity of automobile.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
In foaming concentrate of the present invention, each constituent mass per-cent is: linear low density polyethylene resin 30-60%; Second Warburg Pincus rubber 10-40%; Terpolymer EP rubber 5-15%; Olefin type elastomer resin 5-20%; Cis-1,4-polybutadiene rubber 2-10%; Nucleator 3-5%.
The each constituent mass per-cent of foamed material mixture of the present invention is: foaming concentrate 65-80%; Whipping agent 15-30%; Frothing aid 1-3%; Linking agent is 1.2-5%; Crosslinking coagent 1.5-5%.
Composition main in foaming concentrate is linear low density polyethylene (LLDPE), requires that density is 0.9200-0.9240g/cm 3, melt flow rate (MFR) is 4.5-7.5g/10min, and elongation at break is more than or equal to 100%, and fracture tensile strength is more than or equal to 8MPa, and shore hardness is more than or equal to 42, and fusing point is 106-111 DEG C, and Vicat softening point is more than or equal to 86 DEG C.Second Warburg Pincus rubber (EVM) requires that VA content is 50 ± 1.5%, and mooney viscosity is 27 ± 4ML100 DEG C of 1+4.Olefin type elastomer (POE) requires that melt flow rate (MFR) is greater than 8g/10min, and VA content is greater than 11%.Submember terpolymer EP rubber (EPDM) requires that mooney viscosity is 28ML100 DEG C of 1+4, and the rare content of second is 57%, and Third monomer kind is ENB, Third monomer content 7.9%.Cis-1,4-polybutadiene rubber requires that mooney viscosity is 45ML100 DEG C of 1+4, and ash content is≤0.3%.
Nucleator of the present invention is talcum powder.Talcum powder requires that order number is 800, and proportion is at 2.7-2.8g/cm 3.
Whipping agent of the present invention is the one in azo dimethylamine (AC), 4,4-disulfonyl hydrazide diphenyl ethers (OBSH).Azo dimethylamine (AC) requires decomposition temperature 160 ± 3 DEG C, gas forming amount 180 ± 5ml/g (STP), median size 4.5-6.5 μm.4,4-disulfonyl hydrazide diphenyl ether (OBSH) requires decomposition temperature 140 ± 3 DEG C, and gas forming amount is greater than 129ml/g (STP).
Frothing aid of the present invention is one or both in zinc oxide (ZNO), stearic acid.Zinc oxide (ZNO) requires zinc oxide>=90%, specific surface area>=25m 2/ g, plumbous oxide≤0.01%, manganese oxide≤0.01%, cupric oxide≤0.005%, hydrochloric acid insoluble substance≤0.1%, burning decrement≤5-10%, moisture %≤0.7, screenings (45um)≤0.35%, tap density≤0.4g/ml.Stearic acid requires that fusing point is 69.6 ± 2 DEG C, and boiling point is 232 ± 2 DEG C (2.0kPa), relative density 0.9408g/cm 3, decomposition temperature is 360 ± 2 DEG C, and flash-point is 220.6 DEG C.
Linking agent of the present invention is the one in peroxide diisopropylbenzene(DIPB) (DCP), dual-tert-butyl peroxy isopropyl base benzene (BIPB).Peroxide diisopropylbenzene(DIPB) (DCP) requires that fusing point is 41 ~ 42 DEG C, relative density 1.082, and decomposition temperature is 120 ~ 125 DEG C.Dual-tert-butyl peroxy isopropyl base benzene (BIPB) requires theoretical active oxygen content 9.45%, decomposition temperature 182 DEG C (1 minute transformation period).
Crosslinking coagent of the present invention is the one in trimethylolpropane trimethacrylate (TMPTMA), cyanacrylate (TAIC).Trimethylolpropane trimethacrylate (TMPTMA) requires proportion (25 DEG C) 1.06 ~ 1.07g/cm 3, viscosity (cps is at 25 DEG C) 35 ~ 50, surface tension (dyne/cm) 32.2.Stopper: (MEHQ, ppm) 50 ~ 400.Cyanacrylate (TAIC) requires proportion: 1.155g/cm 3(30 DEG C), specific heat 0.6(40 DEG C), fusing point 17-21 DEG C, flash-point 355 DEG C, viscosity 83 ± 3 centipoise (30 DEG C), boiling point 144 DEG C/3mmHg; 297 DEG C/N2,760mm/Hg.
This foam material in addition to the above components, also other auxiliary agent can be inserted in foamed material, as scorch retarder, anti-aging agent, sulphur etc., other additive dosage (mass percent) is 0.2%-5%(wherein scorch retarder 0.1%-1% anti-aging agent 1%-2%, sulphur 1%-1.5%).
Major equipment XK-250 type Banbury mixer, XK-360 type opening rubber mixing machine, WF-5.5K temperature control frequency conversion forcing machine that the present invention adopts.
Embodiment 1: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
The mass percent of each component of foaming concentrate: linear low density polyethylene resin 40.4%; Second Warburg Pincus rubber 20.2%; Terpolymer EP rubber 15.15%; Olefin type elastomer resin 10.1%; Cis-1,4-polybutadiene rubber 10.1%; Talcum powder 4.04%.
Foaming concentrate preparation process: first precise linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemical) 20Kg by mass percentage, second Warburg Pincus rubber (trade mark 500HV Bayer Bitterfeld GmbH) 10Kg, olefin type elastomer resin (trade mark VM3000 Exxon Mobil) 5Kg, cis-1,4-polybutadiene rubber (trade mark BR9000 Gaoqiao Petrochemical Company petrochemical industry) 5Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 7.5Kg and talcum powder (800 order) 2Kg, banburying is carried out in XK-250 type Banbury mixer, feeding sequence is first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin carries out banburying, the banburying time is 5 minutes, be vented 3 times, finally cis-1,4-polybutadiene rubber and terpolymer EP rubber are dropped in Banbury mixer, banburying is discharge after 3 minutes, be foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 78.57%; Azo dimethylamine 15.87%; Zinc oxide 0.79%; Stearic acid 0.24%; Peroxide diisopropylbenzene(DIPB) 1.75%; Trimethylolpropane trimethacrylate (TMPTMA) 2.28%; Sulphur 0.4%.
Foam material mixing process: first accurately take foaming concentrate 24.75Kg input XK-360 type opening rubber mixing machine by mass percentage and open refining, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 5kg respectively, zinc oxide (content >=90%) 0.25Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.075Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.55Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches Chemical Company) 0.75Kg and sulphur 0.125Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3200%, and height multiplying power is 870%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 2: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
When preparation process is identical with embodiment 1 for the percent mass of foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 75.86%, azo dimethylamine 15.33%; Zinc oxide 0.77%; Stearic acid 0.38%; Peroxide diisopropylbenzene(DIPB) 3.07%, trimethylolpropane trimethacrylate (TMPTMA) 3.83%; Sulphur 0.77%.
Foam material mixing process: take 24.75Kg masterbatch input XK-360 type opening rubber mixing machine and begin to pratise, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 5kg respectively, zinc oxide (content >=90%) 0.25Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.125Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 1Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches Chemical Company) 1.25Kg and sulphur 0.25Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3050%, and height multiplying power is 850%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 3: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
When preparation process is identical with embodiment 1 for the percent mass of foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 73.72%; Azo dimethylamine 11.17%; 4,4-disulfonyl hydrazide diphenyl ether (OBSH) 7.45%; Zinc oxide 1.12%; Stearic acid 0.74%; Peroxide diisopropylbenzene(DIPB) 2.23%; Trimethylolpropane trimethacrylate (TMPTMA) 2.98%; Sulphur 0.6%.
Foam material mixing process: take 24.75Kg foaming concentrate input XK-360 type opening rubber mixing machine and begin to pratise, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 3.75kg respectively, 4, 4-disulfonyl hydrazide diphenyl ether (BOSH) (Hangzhou Hai Hong) 2.5kg, frothing aid zinc oxide (content >=90%) 0.375Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches Chemical Company) 1Kg and sulphur 0.2Kg mixes, mixing time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3400%, and height multiplying power is 920%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 4: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
The mass percent of each component of foaming concentrate: linear low density polyethylene resin 50.85%; Second Warburg Pincus rubber 25.42%; Terpolymer EP rubber 8.47%%; Olefin type elastomer resin 8.47%1%; Cis-1,4-polybutadiene rubber 3.39%; Talcum powder 3.39%.
Foaming concentrate preparation process: first precise linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemical) 20Kg by mass percentage, linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemical) 10Kg, second Warburg Pincus rubber (trade mark 500HV Bayer Bitterfeld GmbH) 15Kg, olefin type elastomer resin (trade mark VM3000 Exxon Mobil) 5Kg, cis-1,4-polybutadiene rubber (trade mark BR9000 Gaoqiao Petrochemical Company) 2Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 5Kg and talcum powder (800 order) 2Kg, banburying is carried out in XK-250 type Banbury mixer, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin carries out banburying, the banburying time is 5 minutes, be vented 3 times, finally cis-1,4-polybutadiene rubber and terpolymer EP rubber are dropped in Banbury mixer, banburying is discharge after 3 minutes, be foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 72.25%; Azo dimethylamine 21.43%; Zinc oxide 0.92%; Stearic acid 0.61%; Peroxide diisopropylbenzene(DIPB) 1.84%; Trimethylolpropane trimethacrylate (TMPTMA) 2.45%; Sulphur 0.49%.
Foam material mixing process: first accurately take foaming concentrate 29.5Kg input XK-360 type opening rubber mixing machine by mass percentage and open refining, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg respectively, zinc oxide (content >=90%) 0.375Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches Chemical Company) 1Kg and sulphur 0.2Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 80-100 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3650%, and height multiplying power is 895%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 5: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
The mass percent of each component of foaming concentrate: linear low density polyethylene resin 62.5%; Second Warburg Pincus rubber 15.63%; Terpolymer EP rubber 7.81%; Olefin type elastomer resin 7.81%; Cis-1,4-polybutadiene rubber 3.13%; Talcum powder 3.13%.
Foaming concentrate preparation process: first precise linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemical) 40Kg by mass percentage, second Warburg Pincus rubber (trade mark 500HV Bayer Bitterfeld GmbH) 10Kg, olefin type elastomer resin (trade mark VM3000 Exxon Mobil) 5Kg, cis-1,4-polybutadiene rubber (trade mark BR9000 Gaoqiao Petrochemical Company) 2Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 5Kg and talcum powder (800 order) 2Kg, banburying is carried out in XK-250 type Banbury mixer, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin carries out banburying, the banburying time is 5 minutes, be vented 3 times, finally cis-1,4-polybutadiene rubber and terpolymer EP rubber are dropped in Banbury mixer, banburying is discharge after 3 minutes, be foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 73.86%; Azo dimethylamine 20.2%; Zinc oxide 0.87%; Stearic acid 0.58%; Peroxide diisopropylbenzene(DIPB) 1.73%; Trimethylolpropane trimethacrylate (TMPTMA) 2.31%; Sulphur 0.46%.
Foam material mixing process: first accurately take foaming concentrate 32Kg input XK-360 type opening rubber mixing machine by mass percentage and open refining, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg respectively, zinc oxide (content >=90%) 0.375Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches Chemical Company) 1Kg and sulphur 0.2Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3550%, and height multiplying power is 882%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 6, automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
The mass percent of each component of foaming concentrate: linear low density polyethylene resin 64.75%; Second Warburg Pincus rubber 14.39%; Terpolymer EP rubber 7.19%; Olefin type elastomer resin 7.19%; Cis-1,4-polybutadiene rubber 2.88%; Talcum powder 3.6%.
Foaming concentrate preparation process: first precise linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemical) 25Kg by mass percentage, linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemical) 20Kg, second Warburg Pincus rubber (trade mark 500HV Bayer Bitterfeld GmbH) 10Kg, olefin type elastomer resin (trade mark VM3000 Exxon Mobil) 5Kg, cis-1,4-polybutadiene rubber (trade mark BR9000 Gaoqiao Petrochemical Company) 2Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 5Kg and talcum powder (800 order) 2.5Kg, banburying is carried out in XK-250 type Banbury mixer, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin carries out banburying, the banburying time is 5 minutes, be vented 3 times, finally cis-1,4-polybutadiene rubber and terpolymer EP rubber are dropped in Banbury mixer, banburying is discharge after 3 minutes, be foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 73.95%; Azo dimethylamine 18.62%; Zinc oxide 1.06%; Stearic acid 0.53%; Dual-tert-butyl peroxy isopropyl base benzene (BIPB) 2.13%; Cyanacrylate (TAIC) 3.19%; Sulphur 0.53%.
Foam material mixing process: first accurately take foaming concentrate 34.75Kg input XK-360 type opening rubber mixing machine by mass percentage and open refining, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg respectively, zinc oxide (content >=90%) 0.5Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.25Kg, dual-tert-butyl peroxy isopropyl base benzene (BIPB) section Ademilson chemical industry) 1Kg, cyanacrylate (TAIC) (Shanghai Fang Rui reaches Chemical Company) 1.5Kg and sulphur 0.25Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3200%, and height multiplying power is 920%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
Embodiment 7: automobile cavity low-smoke and flame retardant modified polyvinyl resin foam material is preparation method carry out according to following steps:
The mass percent of each component of foaming concentrate: linear low density polyethylene resin 30.46%; Second Warburg Pincus rubber 30.46%; Terpolymer EP rubber 5.08%; Olefin type elastomer resin 5.08%; Cis-1,4-polybutadiene rubber 2.03%; Talcum powder 3.05%.
Foaming concentrate preparation process: first precise linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemical) 30Kg by mass percentage, second Warburg Pincus rubber (trade mark 500HV Bayer Bitterfeld GmbH) 30Kg, olefin type elastomer resin (trade mark VM3000 Exxon Mobil) 5Kg, cis-1,4-polybutadiene rubber (trade mark BR9000 Gaoqiao Petrochemical Company) 2Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 5Kg and talcum powder (800 order) 3Kg, banburying is carried out in XK-250 type Banbury mixer, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin carries out banburying, the banburying time is 5 minutes, be vented 3 times, finally cis-1,4-polybutadiene rubber and terpolymer EP rubber are dropped in Banbury mixer, banburying is discharge after 3 minutes, be foaming concentrate.
The each constituent mass per-cent of foamed material mixture: foaming concentrate 76.16%; Azo dimethylamine 17.77%; Zinc oxide 1.52%; Stearic acid 0.51%; Dual-tert-butyl peroxy isopropyl base benzene (BIPB) 1.52%; Cyanacrylate (TAIC) 2.03%; Sulphur 0.51%.
Foam material mixing process: first accurately take foaming concentrate 37.5Kg input XK-360 type opening rubber mixing machine by mass percentage and open refining, add azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg respectively, zinc oxide (content >=90%) 0.75Kg, stearic acid (fusing point 69.6 ± 2 DEG C) 0.25Kg, dual-tert-butyl peroxy isopropyl base benzene (BIPB) (section's Ademilson chemical industry) 0.75Kg, cyanacrylate (TAIC) (Shanghai Fang Rui reaches Chemical Company) 1Kg and sulphur 0.25Kg mixes, the mixed time is 15 minutes, the temperature of two rod mill controls at 90 DEG C, time mixing, two rod spacing is 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out material thin-pass 3 times on two rod, then bottom sheet cooling.The width of bottom sheet is 5cm, and thickness is 3cm.The sheet material of last extrusion moulding under WF-5.5K temperature control frequency conversion extruder temperature is 90 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
Through inspection, the foam material surface no-sundries after extruding, smooth without burr, toast 15 minutes at 180 DEG C of baking ovens, the volume expansion ratio of foam material is 3050%, and height multiplying power is 970%.Light the material after expansion with gas fire, flame height is knock down the flame after 38mm, 10s, and expanding material is from putting out.
After testing, the foam material surface luster zero defect that above embodiment is prepared, size is normal, without collapsing.When 140-180 DEG C, height multiplying power >=800%, expansion ratio is more than 3000%.Reach the low cigarette, fire-retardant of foam material expection, foaming rear surface is soft and without hard excellent effect of separating.

Claims (8)

1. an automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method, it is characterized in that, the method is carried out according to following steps:
Step one: plastic banbury mixer prepares foaming concentrate
Linear low density polyethylene resin, second Warburg Pincus rubber, terpolymer EP rubber, olefin type elastomer resin, cis-1,4-polybutadiene rubber and nucleator are fed intake in order: first linear low density polyethylene resin is dropped into Banbury mixer, then nucleator is added, when banburying temperature rises to 120 DEG C, add second Warburg Pincus rubber and olefin type elastomer resin, the banburying time is 4-8 minute, be vented 2-5 time, again terpolymer EP rubber and cis-1,4-polybutadiene rubber are dropped into Banbury mixer, the banburying time is 2-5 minute, last discharge, is foaming concentrate;
Step 2: foamed material mixture is prepared in mill
The foaming concentrate prepared through step one and whipping agent, frothing aid, linking agent, crosslinking coagent are entered mill mixing 10-20 minute, and mixing temperature controls at 80-100 DEG C;
Step 3: the foamed material mixture prepared through step 2 is sent into forcing machine, and the sheet material of extrusion moulding under extruder temperature is 80-100 DEG C of processing condition, is automobile cavity low-smoke and flame retardant modified poly ethylene foam material.
2. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 1, it is characterized in that, in the foaming concentrate described in step one, each constituent mass per-cent is: linear low density polyethylene resin 30-60%; Second Warburg Pincus rubber 10-40%; Terpolymer EP rubber 5-15%; Olefin type elastomer resin 5-20%; Cis-1,4-polybutadiene rubber 2-10%; Nucleator 3-5%.
3. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 1, it is characterized in that, each constituent mass per-cent of the foamed material mixture described in step 2 is: foaming concentrate 65-80%; Whipping agent 15-30%; Frothing aid 1-3%; Linking agent is 1.2-5%; Crosslinking coagent 1.5-5%.
4. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 2, it is characterized in that, described nucleator is talcum powder.
5. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 3, it is characterized in that, described whipping agent is the one in Cellmic C 121,4,4-disulfonyl hydrazide diphenyl ethers.
6. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 3, is characterized in that, described frothing aid is one or both in zinc oxide, stearic acid.
7. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 3, is characterized in that, described linking agent is the one in dicumyl peroxide, dual-tert-butyl peroxy isopropyl base benzene.
8. a kind of automobile cavity low-smoke and flame retardant modified poly ethylene foam material preparation method according to claim 3, it is characterized in that, described crosslinking coagent is the one in trimethylolpropane trimethacrylate, cyanacrylate.
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