CN103613834A - Preparation method of low-smoke flame-retardant modified polyethylene foaming material for cavity of automobile - Google Patents

Preparation method of low-smoke flame-retardant modified polyethylene foaming material for cavity of automobile Download PDF

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CN103613834A
CN103613834A CN201310579753.8A CN201310579753A CN103613834A CN 103613834 A CN103613834 A CN 103613834A CN 201310579753 A CN201310579753 A CN 201310579753A CN 103613834 A CN103613834 A CN 103613834A
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rubber
smoke
foaming
low
foam material
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CN103613834B (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

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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a preparation method of a low-smoke flame-retardant modified polyethylene foaming material for a cavity of an automobile. The method comprises the steps: firstly, preparing a foaming masterbatch by using a plastic mixer, that is, placing linear low density polyethylene resin and a nucleating agent into an internal mixer, adding levapren rubber and olefin elastomer resin to be internally mixed, then, internally mixing ethylene-propylene-diene rubber and butadiene rubber in the internal mixer, and finally, discharging to obtain the foaming masterbatch; and then, preparing a foaming material mixture by using an open mill, that is, mixing the foaming masterbatch, a foaming promoter, a crosslinking agent and a crosslinking promoter in the open mill, delivering the foaming material mixture into an extruder, and carrying out extrusion molding on the foaming material mixture to form a sheet, i.e., the low-smoke flame-retardant modified polyethylene foaming material for the cavity of the automobile. The foaming material has the height ratio of larger than or equal to 800% and the foaming ratio of over 3000% at the temperature of 140-180 DEG C, so that the expected excellent effects of low smoke, flame retardance and soft and hard-knot-free surface after foaming are achieved, and the environment friendliness and safety of the automobile are improved.

Description

Low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity
Technical field
The present invention relates to the preparation of foam material, relate in particular to low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity.
Background technology
Flourish along with Car Industry, people are not only interested in visual experiences intuitively such as the profile of automobile, colors, and the comfortableness that automobile is brought to us and security are also paid much attention to, and a key point weighing comfort level is exactly vibrations and the noise that automobile produced in the process of moving, so reduce the cavity sympathetic response that automobile produces under steam, reduce automobile cavity inside because circulation of air is extremely important with the noise pollution that vibrations friction produces.And the flame retardant resistance of automobile material therefor also must be paid attention to.
It is material of main part that current automobile cavity is generally taked EVA with foam material, first EVA material does not have flame retardant effect, meets fiery easy firing, and secondly the maximum expansion ratio of EVA material is generally 25 times of left and right, and height multiplying power is generally 5 times of left and right, limited to the complete fillibility contribution of automobile cavity.
Summary of the invention
In view of problem and the defect that above-mentioned prior art exists, the invention provides low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity.The material that adopts 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 that reduces the density after material volume and product foaming.But because material after foaming easily produces cracking and hard solution, easily come off, and product is inflammable, linear low density polyethylene resin can not address these problems well, to realizing height multiplying power, also contribute deficiency in cavity simultaneously.So add terpolymer EP rubber and cis-1,4-polybutadiene rubber in linear low density polyethylene resin, play product foaming rear soft, effect not easy to crack.And add second Warburg Pincus rubber mainly to play two effects: 1. second Warburg Pincus rubber has good flame retardant resistance, can in formula for a product, serve as the effect of fire retardant; 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.Add olefin type elastomer resin to play a part larger for the height multiplying power improving after product foaming.
The technical scheme that the present invention takes is: low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity, it is characterized in that, and the method is carried out according to following steps:
Step 1: plastic banbury mixer is prepared 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 add nucleator, when banburying temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin, the banburying time is 4-8 minute, exhaust 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 of preparing through step 1 and whipping agent, frothing aid, linking agent, crosslinking coagent are entered to mill mixing 10-20 minute, and mixing temperature is controlled at 80-100 ℃;
Step 3: the foamed material mixture of preparing through step 2 is sent into forcing machine, is the sheet material of extrusion moulding under 80-100 ℃ of processing condition at extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Feature of the present invention is, the plastic foamed goods that the foam material that adopts present method to prepare is processed, because its density is little, have been realized car light; This material foam volume is large, can save material cost; Foaming product good with type, is easy to constructing operation; This material has the advantages that unidirectional expansion ratio is large, and height multiplying power >=800%, is conducive to large cavity to be filled.This is one of maximum feature of the present invention.
Low cigarette, the fire-retardant feature that this foam material is realized is different from other foamed products and adds fire retardant, but the anti-flaming function being had by second Warburg Pincus rubber components self realization, the environmental protection and the security that have therefore improved automobile.Thereby reach the filling that meets the large cavity of automobile, intercept the circulation of automobile cavity air, the object to 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%.
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%.
In foaming concentrate, main composition is linear low density polyethylene (LLDPE), and requiring density is 0.9200-0.9240g/cm 3, melt flow rate (MFR) is 4.5-7.5 g/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 ℃, and Vicat softening point is more than or equal to 86 ℃.Second Warburg Pincus rubber (EVM) requires VA content 50 ± 1.5%, and mooney viscosity is 27 ± 4ML100 ℃ of 1+4.Olefin type elastomer (POE) requires melt flow rate (MFR) to be greater than 8 g/10min, and VA content is greater than 11%.It is 28 ML100 ℃ 1+4 that submember terpolymer EP rubber (EPDM) requires mooney viscosity, and the rare content of second is that 57%, the three monomeric species is ENB, the 3rd monomer content 7.9%.It is 45 ML100 ℃ 1+4 that cis-1,4-polybutadiene rubber requires mooney viscosity, and ash content is≤0.3%.
Nucleator of the present invention is talcum powder.It is 800 that talcum powder requires order number, and proportion is at 2.7-2.8g/cm 3.
Whipping agent of the present invention is azo dimethylamine (AC), 4, a kind of in 4-disulfonyl hydrazide diphenyl ether (OBSH).Azo dimethylamine (AC) requires 160 ± 3 ℃ of decomposition temperatures, gas forming amount 180 ± 5ml/g (STP), median size 4.5-6.5 μ m.4,4-disulfonyl hydrazide diphenyl ether (OBSH) requires 140 ± 3 ℃ of decomposition temperatures, and gas forming amount is greater than 129 ml/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.It is 69.6 ± 2 ℃ that stearic acid requires fusing point, and boiling point is 232 ± 2 ℃ (2.0kPa), relative density 0.9408g/cm 3, decomposition temperature is 360 ± 2 ℃, flash-point is 220.6 ℃.
Linking agent of the present invention is a kind of in peroxide diisopropylbenzene(DIPB) (DCP), dual-tert-butyl peroxy isopropyl base benzene (BIPB).It is 41～42 ℃ that peroxide diisopropylbenzene(DIPB) (DCP) requires fusing point, relative density 1.082, and decomposition temperature is 120～125 ℃.Dual-tert-butyl peroxy isopropyl base benzene (BIPB) requires theoretical active o content 9.45%, 182 ℃ of decomposition temperatures (1 minute transformation period).
Crosslinking coagent of the present invention is a kind of in trimethylolpropane trimethacrylate (TMPTMA), cyanacrylate (TAIC).Trimethylolpropane trimethacrylate (TMPTMA) requires proportion (25 ℃) 1.06 ~ 1.07 g/cm 3, viscosity (cps is at 25 ℃) 35 ~ 50, surface tension (dyne/cm) 32.2.Stopper: (MEHQ, ppm) 50 ~ 400.Cyanacrylate (TAIC) requires proportion: 1.155 g/cm 3(30 ℃), specific heat 0.6(40 ℃), fusing point 17-21 ℃, 355 ℃ of flash-points, viscosity 83 ± 3 centipoises (30 ℃), 144 ℃/3mmHg of boiling point; 297 ℃/N2,760mm/Hg.
This foam material is except above component, in foamed material, also can insert other auxiliary agent, as scorch retarder, anti-aging agent, sulphur etc., other additive dosage (mass percent) is wherein scorch retarder 0.1%-1% anti-aging agent 1%-2%, sulphur 1%-1.5% of 0.2%-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 carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
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 accurately weigh by mass percentage linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemicals) 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 petrochemical industry) 5Kg, terpolymer EP rubber (trade mark KEP330 Korea S Jin Hu) 7.5Kg and talcum powder (800 order) 2Kg, in XK-250 type Banbury mixer, carry out banburying, feeding sequence is for first dropping into linear low density polyethylene resin and talcum powder, when temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin to carry out banburying, the banburying time is 5 minutes, exhaust 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.
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 by mass percentage foaming concentrate 24.75Kg input XK-360 type opening rubber mixing machine and open refining, add respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 5kg, zinc oxide (content >=90%) 0.25Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.075Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.55Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches chemical company limited) 0.75Kg and sulphur 0.125Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3200%, height multiplying power is 870%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 2: automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
The mass percent of foaming concentrate and preparation process are identical with embodiment 1.
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 respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 5kg, zinc oxide (content >=90%) 0.25Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.125Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 1Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches chemical company limited) 1.25Kg and sulphur 0. 25Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3050%, height multiplying power is 850%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 3: automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
The mass percent of foaming concentrate and preparation process are identical with embodiment 1.
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 respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 3.75kg, 4, 4-disulfonyl hydrazide diphenyl ether (BOSH) (Hangzhou Hai Hong) 2.5kg, frothing aid zinc oxide (content >=90%) 0.375Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches chemical company limited) 1 Kg and sulphur 0. 2Kg mix, mixing time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3400%, height multiplying power is 920%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 4: automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
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 accurately weigh by mass percentage linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemicals) 20Kg, linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemicals) 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, in XK-250 type Banbury mixer, carry out banburying, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin to carry out banburying, the banburying time is 5 minutes, exhaust 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.
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 by mass percentage foaming concentrate 29.5Kg input XK-360 type opening rubber mixing machine and open refining, add respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg, zinc oxide (content >=90%) 0.375Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches chemical company limited) 1Kg and sulphur 0.2Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 80-100 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3650%, height multiplying power is 895%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 5: automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
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 accurately weigh by mass percentage linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemicals) 40Kg, 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, in XK-250 type Banbury mixer, carry out banburying, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin to carry out banburying, the banburying time is 5 minutes, exhaust 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.
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 by mass percentage foaming concentrate 32Kg input XK-360 type opening rubber mixing machine and open refining, add respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg, zinc oxide (content >=90%) 0.375Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.25Kg, peroxide diisopropylbenzene(DIPB) (Shanghai Gaoqiao) 0.75Kg, trimethylolpropane trimethacrylate (TMPTMA) (Shanghai Fang Rui reaches chemical company limited) 1Kg and sulphur 0.2Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3550%, height multiplying power is 882%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 6, and automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
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 accurately weigh by mass percentage linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemicals) 25Kg, linear low density polyethylene resin (trade mark 605 Beijing Yanshan Petrochemicals) 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, in XK-250 type Banbury mixer, carry out banburying, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin to carry out banburying, the banburying time is 5 minutes, exhaust 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.
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 by mass percentage foaming concentrate 34.75Kg input XK-360 type opening rubber mixing machine and open refining, add respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg, zinc oxide (content >=90%) 0.5Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 0.25Kg, dual-tert-butyl peroxy isopropyl base benzene (BIPB) section Ademilson chemical industry) 1Kg, cyanacrylate (TAIC) (Shanghai Fang Rui reaches chemical company limited) 1.5Kg and sulphur 0.25Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3200%, height multiplying power is 920%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
Embodiment 7: automobile cavity carries out according to following steps by low-smoke and flame retardant modified polyvinyl resin foam material preparation method:
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 accurately weigh by mass percentage linear low density polyethylene resin (trade mark 607 Beijing Yanshan Petrochemicals) 30Kg, 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, in XK-250 type Banbury mixer, carry out banburying, feeding sequence is: first drop into linear low density polyethylene resin and talcum powder, when temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin to carry out banburying, the banburying time is 5 minutes, exhaust 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.
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 by mass percentage foaming concentrate 37.5Kg input XK-360 type opening rubber mixing machine and open refining, add respectively azo dimethylamine (trade mark 6000 Hangzhou Hai Hong) 8.75kg, zinc oxide (content >=90%) 0.75Kg, stearic acid (69.6 ± 2 ℃ of fusing points) 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 limited) 1Kg and sulphur 0.25Kg mix, the mixed time is 15 minutes, the temperature of two rod mills is controlled at 90 ℃, when mixing, two rod spacing are 5mm, after mixing, be foamed material mixture.
Foamed material mixture is carried out to material thin-pass 3 times on two rods, then descend sheet cooling.The width of lower is 5cm, and thickness is 3cm.Last is the sheet material of extrusion moulding under 90 ℃ of processing condition at WF-5.5K temperature control frequency conversion extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
Through check, the foam material surface no-sundries after extruding, smooth smooth without burr, 180 ℃ of baking oven bakings 15 minutes, the volume expansion ratio of foam material was 3050%, height multiplying power is 970%.With gas fire, light the material after expansion, flame height is 38mm, knock down the flame after 10s, and expanding material is from putting out.
After testing, the foam material surface luster zero defect that above embodiment prepares, size is normal, without collapsing.In the time of 140-180 ℃, height multiplying power >=800%, expansion ratio is more than 3000%.Reached the low cigarette that foam material is expected, fire-retardant, the excellent effect of foaming rear surface softness and the hard solution of nothing.

Claims (8)

1. a low-smoke and flame retardant modified poly ethylene foam material preparation method for automobile cavity, is characterized in that, the method is carried out according to following steps:
Step 1: plastic banbury mixer is prepared 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 add nucleator, when banburying temperature rises to 120 ℃, add second Warburg Pincus rubber and olefin type elastomer resin, the banburying time is 4-8 minute, exhaust 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 of preparing through step 1 and whipping agent, frothing aid, linking agent, crosslinking coagent are entered to mill mixing 10-20 minute, and mixing temperature is controlled at 80-100 ℃;
Step 3: the foamed material mixture of preparing through step 2 is sent into forcing machine, is the sheet material of extrusion moulding under 80-100 ℃ of processing condition at extruder temperature, is low-smoke and flame retardant modified poly ethylene foam material for automobile cavity.
2. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 1, is characterized in that, in the foaming concentrate described in step 1, 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. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 1, 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. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 2, is characterized in that, described nucleator is talcum powder.
5. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 3, is characterized in that, described whipping agent is azo dimethylamine, 4, a kind of in 4-disulfonyl hydrazide diphenyl ether.
6. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 3, is characterized in that, described frothing aid is one or both in zinc oxide, stearic acid.
7. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 3, is characterized in that, described linking agent is a kind of in peroxide diisopropylbenzene(DIPB), dual-tert-butyl peroxy isopropyl base benzene.
8. low-smoke and flame retardant modified poly ethylene foam material preparation method for a kind of automobile cavity according to claim 3, is characterized in that, described crosslinking coagent is a kind of in trimethylolpropane trimethacrylate, cyanacrylate.
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