CN103739946A - High-impact high-stiffness polypropylene rotational molding material and preparation method thereof - Google Patents
High-impact high-stiffness polypropylene rotational molding material and preparation method thereof Download PDFInfo
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- CN103739946A CN103739946A CN201310668359.1A CN201310668359A CN103739946A CN 103739946 A CN103739946 A CN 103739946A CN 201310668359 A CN201310668359 A CN 201310668359A CN 103739946 A CN103739946 A CN 103739946A
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L23/12—Polypropene
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- 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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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- 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
- B29B9/00—Making granules
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- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B29C2948/00—Indexing scheme relating to extrusion moulding
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- B29C2948/92695—Viscosity; Melt flow index [MFI]; Molecular weight
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- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
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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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- 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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- C08L2205/00—Polymer mixtures characterised by other features
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- 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
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Abstract
The invention relates to a high-impact high-stiffness polypropylene rotational molding material and a preparation method thereof. The rolling plastic rotational molding material comprises the following raw materials: by weight, 100 parts of polypropylene, 0-30 parts of polyethylene, 0-0.1 part of a crosslinking agent, 0-0.15 part of an auxiliary crosslinking agent, 1-10 parts of an elastomer, 0.1-0.5 part of an antioxidant, 0-10 parts of a nano filler, 0.1-0.5 part of a dispersing lubricant and 0-0.4 part of a surface treatment agent. According to the invention, the crosslinkable polyethylene is added in a polypropylene melt mixing process for melt curing to obtain the high-impact high-stiffness polypropylene modified rotational molding material with a semi interpenetrating network structure, and the high-impact high-stiffness polypropylene modified rotational molding material can meet the material requirements of vehicles and other different fields. The curing reaction of the polyethylene belongs to the in situ curing, the material has the unique semi interpenetrating network structure, different components are mutually bitten or buckled, the compatibility between the polyethylene and polypropylene resin can be improved, and the performance advantages of the both are full played.
Description
Technical field
The present invention relates to rotational moulding material and rotational molding technique, particularly a kind of high resistance rigid polypropylene rotational moulding material and preparation method thereof of leaping high.
Background technology
Rotational molding technique is because be applicable to moulding Large Hollow Container, and product internal stress is very little, in China, has obtained development rapidly, and product is increasingly extensive.Rotational molding technique also becomes increasingly abundant to the consumption of raw material and kind demand, the kind of the rotational moulding raw material that current domestic each producer is used is single, more than 99% rotomoulded articles raw material is PE, wherein 95% is the linear low density polyethylene (LLDPE) of rotational molding grade, because it is good that linear low density polyethylene has stress crack resistant, shock resistance is superior, and the advantage such as short and easy abrasive dust of shaping cycle is considered to be rich in most in rotational moulding industry the raw material of development prospect.Yet the development along with rotomoulding apparatus, technology, rotational moulding from traditional Large Hollow Container Application Areas to small piece, corrosion-proof lining, automobile, equipment component development, in these fields, because linear low density polyethylene is corrosion-resistant, wear-resisting, impermeable, the shortcoming of heat-resisting creep properties aspect, has limited the application of linear low density polyethylene; Moreover because domestic rotational molding grade LLDPE raw material has approached middle density category density, its resistance to low temperature is restriction to some extent also, simultaneously its also Shortcomings aspect the mechanical properties such as bending elastic modulus, flexural strength, tensile strength, is mainly applicable to the civilian goods of low grade under normal temperature.For head it off, domestic many enterprises have carried out the modification of LLDPE to improve its mechanical property, thermotolerance and Integrated using performance.
CN101735505A discloses a kind of rotational moulding and wear-resistant polyolefin resin and preparation method thereof, this patent be take linear low density polyethylene, high density polyethylene(HDPE) or polypropylene as body material, by adding mineral filler, ultrahigh molecular weight polyethylene(UHMWPE) and Lubrication Composition, improve the wear resisting property of material.CN101265343A has announced the preparation method of a kind of high-strength, high-ductility, the high rotational moulding PP Pipe Compound that flows, it is raw material that this patent be take linear low density polyethylene and irradiation high density polyethylene(HDPE), by adding nano imvite and nucleator to improve tensile strength and the shock strength of material.CN102816372A has announced a kind of preparation method of high-impact weathering resistance automobile rotational moulding plastic tool box proprietary material, by add elastomerics in the resin of polyethylene basis, UV light absorber etc., improve Long-term Anti aging and the resistance to low temperature of material, can be used for extremely frigid zones automobile plastic work box.In foregoing invention, although the method that polyethylene is carried out to physically modified can improve its machinery, the performance such as anti-aging to a certain extent, but the intrinsic attribute of polyethylene has determined that the space of the improvement in performance of material is limited, in particular application, high temperature for example, in the applied environments such as high rigidity, modified poly ethylene also cannot meet the demands.CN1580165A has announced a kind of application of high-temperature resistant anti-corrosive polyolefin compositions powder, by introduce linking agent and polypropylene in polyethylene, improved the anticorrosion and resistance to elevated temperatures of material, but this material is because contain a large amount of polar groups, therefore be mainly used in top layer corrosion-resistant field, and be not suitable for the overall plastic product of preparation.Along with the development of rotational molding technique and equipment, there is increasing rotational moulding resin, polycarbonate for example, polypropylene, nylon etc.Compare polyethylene, these material temperature tolerances, rigidity are with the obvious advantage, but cold resistance can and creep-resistant property poor, the application of rotational moulding field seldom, can not be directly used in the rotational moulding products such as automobile.
Summary of the invention
Problem and defect in view of above-mentioned prior art existence, the invention provides a kind of high resistance rigid polypropylene rotational moulding material and preparation method thereof of leaping high, the polypropylene rotational moulding material of taking present method to prepare, both guaranteed that material had higher rigidity, there is remarkable impact property and heat resisting and pressure resisting performance simultaneously, can be applicable to the rotational moulding products such as military products case, automobile urea box.
The present invention solves the technical scheme that above technical problem takes: a kind of high resistance rigid polypropylene rotational moulding material of leaping high, it is characterized in that, by forming according to the raw material of mass fraction metering below:
Polypropylene 100
Polyethylene 0-30
Linking agent 0-0.1
Additional crosslinker 0-0.15
Elastomerics 1-10
Oxidation inhibitor 0.1-0.5
Nano level stopping composition 0-10
Dispersed lubricant 0.1-0.5
Surface treatment agent 0-0.4.
The leap high preparation method of rigid polypropylene rotational moulding material of a kind of high resistance of the present invention, is characterized in that, described preparation method carries out according to following steps:
Step 1: drying treatment is to moisture content lower than 600ppm in advance by polyethylene, and abrasive dust 30-50 order is standby.
Step 2: linking agent and additional crosslinker are weighed by certain mass umber, and mix 2-10 minute in magnetic stirrer; Mixed linking agent/additional crosslinker is mixed after 5-10 minute with the polyethylene after abrasive dust in mixing machine, be prepared into the sealing of polyethylene powder standby.
Step 3: surface treatment agent and nano level stopping composition are pressed to certain mass umber, in mixing machine, mix 2-8 minute, the nano level stopping composition that is mixed with surface treatment agent is mixed to 5-10 minute with the polyethylene powder of preparing in the polypropylene of weighing by certain mass umber, elastomerics, oxidation inhibitor, dispersed lubricant and step 2 in mixing machine, then at extrusion temperature, be 180-240 ℃, screw speed is extruding pelletization under 200-500rpm processing condition, after extruding pelletization, abrasive dust 50-100 order, and powder is dried to moisture content lower than 600ppm.
Advantage of the present invention is: the present invention adds crosslinkable polyethylene in polypropylene fusion mixing process, carry out melting and solidification, obtain a kind of polypropylene modification rotational moulding material with half interpenetrating network structure, high strength, high tenacity, can meet the requirement of the different field such as automobile to material.
In the present invention, poly curing reaction belongs to in-situ solidifying, and material has distinctive half interpenetrating network structure, and between different components, button is stung mutually, can improve the consistency between polyethylene and acrylic resin, gives full play to the advantage in both performances.
Embodiment
Below in conjunction with embodiment, the invention will be further described: the present invention adopts the doubly air-cooled tie rod twin screw extruder of grand CTE-65 of Nanjing section.
Polypropylene of the present invention is selected a kind of or two kinds of combinations in homo-polypropylene, Co-polypropylene.
Polyethylene of the present invention is selected a kind of or combination in linear low density polyethylene, high density polyethylene(HDPE), and its melting index is 2-20g/10min.
Linking agent of the present invention is peroxide type linking agent, selects 2,5-dimethyl-2, two (t-butyl peroxy) hexanes of 5-, bis(2，4-dichlorobenzoyl)peroxide, peroxidation two (4-toluyl), dicumyl peroxide, di-tert-butyl peroxide isopropyl benzene, 1,1-di-t-butyl methyl-3, one or more in 5,5-trimethyl-cyclohexane.
Additional crosslinker of the present invention is cyanacrylate, triallylcyanurate, one or more in trimethylolpropane trimethacrylate.
Elastomerics of the present invention is selected styrene-butadiene copolymer, styrene-ethylene-butadienecopolymer, ethylene-octene copolymer, ethylene-vinyl acetate copolymer, ethylene-propylene copolymer, polyurethane elastomer, one or several in ethylene-acrylic acid copolymer.
Oxidation inhibitor of the present invention is the composite antioxidant that phosphite ester kind antioxidant and Hinered phenols antioxidant form, and wherein phosphite ester kind antioxidant and Hinered phenols antioxidant mix by weight 1:0.3～1:0.7.
Nano level stopping composition of the present invention is selected nano-calcium carbonate, nanomete talc powder, nano-sized magnesium hydroxide, nano-aluminum hydroxide, nano imvite, nano-silicon lime stone, one or several in nano kaoline.
Surface treatment agent of the present invention is selected 3-triethoxysilyl-1-propylamine, γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, stearic acid, titanic acid ester, Aluminate, one or several mixing in zirconate.
Dispersed lubricant of the present invention is selected ethylene bis stearamide, polyethylene wax, montanic acid, calcium stearate, one or several mixing in stearic acid.
Embodiment mono-: a kind of high resistance is leapt high rigid polypropylene rotational moulding material by forming according to the raw material of mass fraction metering below:
Polypropylene 100
Ethylene-octene copolymer 5
Composite antioxidant 0.4
Nanomete talc powder 5
Ethylene bis stearamide 0.4
γ-aminopropyl triethoxysilane 0.1.
Wherein composite antioxidant is mixed by weight 1:0.3 by phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010.
The leap high preparation method of rigid polypropylene rotational moulding material carries out according to following steps a kind of high resistance: 0.1 part of γ-aminopropyl triethoxysilane is mixed 5 minutes with 5 parts of nanomete talc powders in high-speed mixer; The nanomete talc powder of γ-aminopropyl triethoxysilane and the polypropylene of 100 parts, the ethylene-octene copolymer of 5 parts, 0.4 part of composite antioxidant, 0.4 part of ethylene bis stearamide will be mixed with, in middling speed mixing machine, mix 6 minutes, then at extrusion temperature, it is 230 ℃, screw speed is extruding pelletization under 300rpm processing condition, after extruding pelletization, abrasive dust 60 orders, and powder is dried to moisture content lower than 600ppm in 80 ℃ of baking ovens.
Embodiment bis-: a kind of high resistance is leapt high rigid polypropylene rotational moulding material by forming according to the raw material of mass fraction metering below:
Polypropylene 100
High density polyethylene(HDPE) 25
2,5-dimethyl-2, two (t-butyl peroxy) hexanes 0.04 of 5-
Cyanacrylate 0.06
Ethylene-octene copolymer 5
Composite antioxidant 0.3
Ethylene bis stearamide 0.2.
Wherein composite antioxidant is mixed by weight 1:0.5 by phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010.
The leap high preparation method of rigid polypropylene rotational moulding material carries out according to following steps a kind of high resistance:
Step 1: be that in the baking oven of 80 ℃, drying treatment is to moisture content lower than 600ppm at design temperature in advance by high density polyethylene(HDPE), abrasive dust 50 orders are standby.
Step 2: by 0.04 part 2,5-dimethyl-2, two (t-butyl peroxy) hexanes of 5-and 0.06 part of cyanacrylate mix 2 minutes in magnetic stirrer; By mixed 2,5-dimethyl-2, two (t-butyl peroxy) hexanes of 5-and 0.06 part of cyanacrylate mix after 5 minutes in middling speed mixing machine with the polyethylene after abrasive dust, are prepared into polyethylene powder and seal standby.
Step 3: the polyethylene powder of preparing in the polypropylene of 100 parts, the ethylene-octene copolymer of 5 parts, 0.3 part of composite antioxidant, 0.2 part of ethylene bis stearamide and step 2 is mixed 5 minutes in middling speed mixing machine, then at extrusion temperature, it is 220 ℃, screw speed is extruding pelletization under 250rpm processing condition, after extruding pelletization, abrasive dust 60 orders, and powder is dried to moisture content lower than 600ppm in 80 ℃ of baking ovens.
Embodiment tri-: a kind of high resistance is leapt high rigid polypropylene rotational moulding material by forming according to the raw material of mass fraction metering below:
Polypropylene 100
High density polyethylene(HDPE) 12.5
Linear low density polyethylene 12.5
Dicumyl peroxide 0.04
Cyanacrylate 0.06
Ethylene-octene copolymer 6
Composite antioxidant 0.3
Nanomete talc powder 8
Ethylene bis stearamide 0.4
γ-aminopropyl triethoxysilane 0.2.
Wherein composite antioxidant is mixed by weight 1:0.7 by phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010.
The leap high preparation method of rigid polypropylene rotational moulding material carries out according to following steps a kind of high resistance:
Step 1: be that in the baking oven of 80 ℃, drying treatment is to moisture content lower than 600ppm at design temperature in advance by 12.5 parts of high density polyethylene(HDPE)s and 12.5 parts of linear low density polyethylenes, abrasive dust 50 orders are standby.
Step 2: 0.04 part of dicumyl peroxide and 0.06 part of cyanacrylate are mixed 2 minutes in magnetic stirrer; Mixed dicumyl peroxide and cyanacrylate are mixed after 5 minutes in middling speed mixing machine with the polyethylene after abrasive dust, be prepared into the sealing of polyethylene powder standby.
Step 3: by 0.2 part of γ-aminopropyl triethoxysilane and 8 parts of nanomete talc powders at height
In speed mixing machine, mix 5 minutes, the polyethylene powder of preparing in the nanomete talc powder that is mixed with γ-aminopropyl triethoxysilane and the polypropylene of 100 parts, the ethylene-octene copolymer of 6 parts, 0.3 part of composite antioxidant, 0.4 part of ethylene bis stearamide and step 2 is mixed 6 minutes in middling speed mixing machine, then at extrusion temperature, it is 230 ℃, screw speed is extruding pelletization under 300rpm processing condition, after extruding pelletization, abrasive dust 60 orders, and powder is dried to moisture content lower than 600ppm in 80 ℃ of baking ovens.
The performance index of above three embodiment are in Table 1 after testing.
Table 1
As can be seen from the above table, the polypropylene rotational moulding material that adopts present method to be prepared into is compared with rotation molding polyethylene, has higher rigidity and hardness, and impact property is excellent, can meet the requirement of multiple rotomoulded articles moulding process and use properties.
Claims (11)
1. the high resistance rigid polypropylene rotational moulding material of leaping high, is characterized in that, by forming according to the raw material of mass fraction metering below:
Polypropylene 100
Polyethylene 0-30
Linking agent 0-0.1
Additional crosslinker 0-0.15
Elastomerics 1-10
Oxidation inhibitor 0.1-0.5
Nano level stopping composition 0-10
Dispersed lubricant 0.1-0.5
Surface treatment agent 0-0.4.
2. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, is characterized in that, described polypropylene is selected a kind of or two kinds of combinations in homo-polypropylene, Co-polypropylene.
3. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, is characterized in that, described polyethylene is selected a kind of or combination in linear low density polyethylene, high density polyethylene(HDPE), and its melting index is 2-20g/10min.
4.
bis(2，4-dichlorobenzoyl)peroxide, peroxidation two (4-toluyl), dicumyl peroxide, di-tert-butyl peroxide isopropyl benzene, 1,1-di-t-butyl methyl-3, one or more in 5,5-trimethyl-cyclohexane.
5. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, is characterized in that, described additional crosslinker is cyanacrylate, triallylcyanurate, one or more in trimethylolpropane trimethacrylate.
6. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, it is characterized in that, described elastomerics is selected styrene-butadiene copolymer, styrene-ethylene-butadienecopolymer, ethylene-octene copolymer, ethylene-vinyl acetate copolymer, ethylene-propylene copolymer, polyurethane elastomer, one or several in ethylene-acrylic acid copolymer.
7. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, it is characterized in that, described oxidation inhibitor is the composite antioxidant that phosphite ester kind antioxidant and Hinered phenols antioxidant form, and wherein phosphite ester kind antioxidant and Hinered phenols antioxidant mix by weight 1:0.3～1:0.7.
8. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, is characterized in that, described nano level stopping composition is selected nano-calcium carbonate, nanomete talc powder, nano-sized magnesium hydroxide, nano-aluminum hydroxide, nano imvite, nano-silicon lime stone, one or several in nano kaoline.
9. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, it is characterized in that, described surface treatment agent is selected 3-triethoxysilyl-1-propylamine, γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, stearic acid, titanic acid ester, Aluminate, one or several mixing in zirconate.
10. a kind of high resistance as claimed in claim 1 rigid polypropylene rotational moulding material of leaping high, is characterized in that, described dispersed lubricant is selected ethylene bis stearamide, polyethylene wax, montanic acid, calcium stearate, one or several mixing in stearic acid.
The leap high preparation method of rigid polypropylene rotational moulding material of 11. 1 kinds of high resistances as claimed in claim 1, is characterized in that, described preparation method carries out according to following steps:
Step 1: drying treatment is to moisture content lower than 600ppm in advance by polyethylene, and abrasive dust 30-50 order is standby;
Step 2: linking agent and additional crosslinker are weighed by certain mass umber, and mix 2-10 minute in magnetic stirrer; Mixed linking agent/additional crosslinker is mixed after 5-10 minute with the polyethylene after abrasive dust in mixing machine, be prepared into the sealing of polyethylene powder standby;
Step 3: surface treatment agent and nano level stopping composition are pressed to certain mass umber, in mixing machine, mix 2-8 minute, the nano level stopping composition that is mixed with surface treatment agent is mixed to 5-10 minute with the polyethylene powder of preparing in the polypropylene of weighing by certain mass umber, elastomerics, oxidation inhibitor, dispersed lubricant and step 2 in mixing machine, then at extrusion temperature, be 180-240 ℃, screw speed is extruding pelletization under 200-500rpm processing condition, after extruding pelletization, abrasive dust 50-100 order, and powder is dried to moisture content lower than 600ppm.
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