CN105801757A - Long-chain-branch high-melt-strength polypropylene resin and preparation method thereof - Google Patents
Long-chain-branch high-melt-strength polypropylene resin and preparation method thereof Download PDFInfo
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- CN105801757A CN105801757A CN201610171207.4A CN201610171207A CN105801757A CN 105801757 A CN105801757 A CN 105801757A CN 201610171207 A CN201610171207 A CN 201610171207A CN 105801757 A CN105801757 A CN 105801757A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/04—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene copolymers
Abstract
The invention discloses a long-chain-branch high-melt-strength polypropylene resin. The long-chain-branch high-melt-strength polypropylene resin is mainly prepared from, by mass, 100 parts of ethylene propylene co-polypropylene, 0.10-2 parts of an antioxidant, 0.05-1 part of a lubricant, 0.05-1 part of an antistatic agent, 0.01-3 parts of a peroxide initiator, 0.01-5 parts of a first grafted monomer and 0.01-5 parts of a second grafted monomer. The first grafted monomer is vinyl end-capped silicone oil, and the second grafted monomer is cycloolefin, styrene or their combination. The invention further discloses a preparation method of the polypropylene resin. The polypropylene resin is high in melt strength and is especially suitable for foaming, blistering, compression molding, film blowing and other applications.
Description
Technical field
The present invention relates to a kind of acrylic resin and preparation method thereof, particularly to a kind of long-chain branch high fused mass strength poly-third
Olefine resin and preparation method thereof.
Background technology
Polypropylene (PP) due to low-density, high-melting-point, chemical stability processing good, nontoxic, easy, better mechanical property, with
And the advantage such as raw material sources are wide, cheap, it has also become in five big general synthetic resins, growth rate is the fastest, new product development
For active kind.But, carry out propylene polymerization with Ziegler-Natta catalyst and metallocene catalyst and typically result in line style knot
The PP of structure, its softening point and fusing point very close to, melting range is shorter, causes its melt strength low and Sag Resistance is poor, seriously limit
The PP application in processing and forming fields such as thermoforming, blow molding and foaming.Therefore, how high melt strength, propylene is prepared
(HMS-PP) concern of people is caused.The melt strength improving polymer by improving the molecular weight of polymer and can increase it
Molecular weight distribution width realizes, it can in addition contain by the modified method of long-branched.Wherein, later approach has the most excellent
Gesture, while improving melt strength, can effectively suppress the growth of viscosity, makes the processability that polymer holding is good
Energy.
Long-chain branch (LCB) in HMS-PP can produce in the course of the polymerization process, it is also possible in post-treatment, initiation grafting produces
Raw.In post-treatment, initiation grafting generally uses reactive extrursion method, its economy simple to operate, is especially suitable for industrialized production, from
And become and prepare the main method that HMS-PP uses at present.Reactive extrursion method is exactly by polypropylene, initiator and multifunctional single group
Body carries out reversal connection in screw extruder and touches, and does not has the interference of suspension media and solvent.But during reactive extrursion, reactant contains
Amount and structure can appreciable impact HMS-PP melt strength, rheological behaviour and the thermodynamic properties thereof etc. prepared.At preparation Gao Rong
During body strength polypropylene, peroxide is often used as initiator.However, studies have shown that, the introducing of peroxide can make poly-third
Alkene occurs to degrade significantly.A large amount of polyacrylic existence of small-molecular-weight can improve the mobility of polymer, but can significantly drop
The mechanical property of oligomerisation of propene.
Summary of the invention
An object of the present invention is to provide a kind of long-chain branch high fused mass strength polypropylene resin, this acrylic resin
Melt strength is high, is particularly well-suited to the application such as foaming, plastic uptake, compression moulding, blown film.
The two of the purpose of the present invention are to provide the preparation method of the acrylic resin of above-mentioned long-chain branch high fused mass strength.
First purpose of the present invention is achieved through the following technical solutions: a kind of long-chain branch high fused mass strength poly-third
Olefine resin, the raw material of main following mass fraction is prepared from:
Ethylene propylene copolymer polypropylene 100 parts
Antioxidant 0.10～2 parts
Lubricant 0.05～1 part
Antistatic additive 0.05～1 part
Peroxide initiator 0.01～3 parts
First grafted monomers 0.01～5 parts
Second grafted monomers 0.01～5 parts；
Described first grafted monomers is vinyl-terminated silicone oil, described second grafted monomers be cycloolefin, styrene or both
Combination.
The polyacrylic melt flow rate (MFR) of ethylene propylene copolymer of the present invention 8～10g/10min, ethylene contents is 7
～10%, such as anti-impact ethylene propylene copolymer polypropylene (ICP) of the EPC30R-H trade mark that Refinery of Maoming Petrochemical Corporation produces.
Antioxidant can improve acrylic resin heat aging property during processing and use.Institute in the present invention
Stating antioxidant is mixed type antioxidant, for Hinered phenols antioxidant and the combination of phosphite ester kind antioxidant.Wherein, Hinered phenols
Between antioxidant and phosphite antioxidant, mass ratio is 1:13:1.
Described Hinered phenols antioxidant is 2,6-di-tert-butyl-4-methy phenol (BHT, 264), four [β-(3,5-bis-
Tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester (antioxidant 1010) and β-(3,5-di-tert-butyl-hydroxy phenyl)
A kind of or both combinations above in propanoic acid octadecyl ester (antioxidant 1076).
Described phosphite antioxidant is trisnonyl phenyl phosphite (TNPP) or tricresyl phosphite (2,4-bis-uncle
Butyl phenyl) ester.
Lubricant of the present invention is one or more the group in calcium stearate, erucyl amide and behenic acid amide
Close.
Antistatic additive of the present invention is polyol fatty acid ester compounds, is selected from sorbitol anhydride monostearate
One or more combination in ester, glyceryl monostearate and single Glyceryl Behenate.
Peroxide initiator of the present invention be selected from 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane,
Di-t-butyl peroxide, cumyl peroxide, benzoyl peroxide, 2,5-dimethyl-2,5-di-tert-butyl peroxide are
One or more combination in alkynes and two tertiary amyl peroxide.
Described vinyl-terminated silicone oil has higher dissolubility to carbon dioxide, when resin is for foam process, can have
Effect improves the foam performance of material.Vinyl-terminated silicone oil is selected from the contents of ethylene vinyl more than 80% in the present invention
Block poly-methyl-silicone oil or ethenyl blocking methyl phenyl silicone oil or a combination of both.Its structural formula such as following formula institute
Show:
As one embodiment of the present of invention, described cycloolefin is cyclopentadiene.
The present invention the second purpose is achieved through the following technical solutions: a kind of long-chain branch high fused mass strength polypropylene tree
The preparation method of fat, by ethylene propylene copolymer polypropylene, antioxidant, lubricant, antistatic additive, peroxide initiator, first
After grafted monomers and the second grafted monomers mix homogeneously, through double screw extruder extruding pelletization, obtain long-chain branch high fused mass strength
Polypropylene granules.
The present invention also can adopt the preparation alternatively realizing long-chain branch high fused mass strength polypropylene resin, i.e. ethylene propylene
Alkene COPP, antioxidant, lubricant, antistatic additive and peroxide initiator in super mixer after mix homogeneously,
Add in double screw extruder, described first grafted monomers and the second grafted monomers from extruder second, third or the 4th add
The throat-fed of material section, melt extrudes pelletize, obtains long-chain branch high fused mass strength polypropylene pellet.
The method have the advantages that
The present invention is resin based on propylene heterophasic copolymer ethylene propylene copolymer polypropylene, adds the antioxygen of certain proportional quantity
Agent, lubricant, antistatic additive, initiator and grafted monomers, carry out extruding pelletization, it is thus achieved that long-branched changes under suitable condition
Property acrylic resin.The introducing of grafted monomers not only increases the melt strength of acrylic resin, and the first grafted monomers second
Thiazolinyl end-blocking silicone oil has higher dissolubility to carbon dioxide, can be effectively improved the foam performance of resin material, make resin have
Good processing characteristics.The introducing of the second grafted monomers can effectively limit peroxide initiator and make the degraded of polymer
With, thus realize keeping the excellent mechanical property of impact copolymer polypropylene while long-chain branch modification.Therefore the drawing money on credit of the present invention
Chain modified polypropylene resin has superior mechanical property and processing characteristics, can be widely applied to foaming, thermoforming, blown film,
In the production technologies such as Extrusion Coating.
Detailed description of the invention
In the present invention, auxiliary agent is carried out with being blended in super mixer of base resin, and Zhangjagang City's bass spy's machinery has
Limit company manufactures, and model is SHR10A；Polymeric aggregate is extruded by double screw extruder, and Nanjing Ke Ya company manufactures, model
TE-35, screw diameter 35mm, draw ratio (L/D) is 48.
Melt Strength Test Method in embodiments of the invention: MODIFIED PP joins in capillary tube, after heating uniform temperature
After melt is extruded from capillary tube, extrusion is acted on by tensile force vertically downward.Rheotnes is by measuring nip rolls
The draw ratio V of institute stress value F and melt determines the melt strength of polymer, tensile stress, transient state tensile viscosity, elongation strain
The draft flowing deformation physical quantitys such as speed.Concrete test condition is as shown in the table:
The polypropylene used in embodiment is ethylene propylene copolymer polypropylene, and the production of this resin uses Spheripol technique, needs
Produce polypropylene with two step compounding technologies, i.e. the first step uses annular-pipe reactor to carry out propylene liquid phase homopolymerization, second step
Fluidized-bed reactor is used to carry out Noblen and vinyl monomer gas phase copolymerization.The generation of copolymer makes final products
Erosion-resisting characteristics is greatly improved, especially the erosion-resisting characteristics under low temperature.In the presence of a catalyst, annular-pipe reactor Stress control is controlled
3.0～3.6MPa, the addition 0.08～0.12% of hydrogen, gaseous ethene addition 7～10%, the polymer powders obtained
Melt flow rate (MFR) 8～10g/10min.Anti-impact ethylene propylene copolymer such as the EPC30R-H trade mark of Refinery of Maoming Petrochemical Corporation's production gathers
Propylene (ICP).
Embodiment 1
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of monostearates
Glyceride, 1.5 grams of benzoyl peroxides, 60 grams of contents of ethylene molar ratios be 96% the poly-methyl-silicone oil of ethenyl blocking and
6 grams of styrene, in stirrer for mixing 20min to uniformly.Feeding the mixture in double screw extruder, screw speed is 60
R/min, rate of feeding is 4.8 kg/h, and the revolution of extruder is set as 15 revs/min.Extruder is divided into four thermals treatment zone, its
In a Heating Zone Temperature be set as 165 DEG C, two Heating Zone Temperature are set as 180 DEG C, and three Heating Zone Temperature are set as 190 DEG C, four
Heating Zone Temperature is set as 190 DEG C, and extruding pelletization obtains long-chain branch high fused mass strength polypropylene resin.Take sample segment to carry out
Performance test and melt strength measure, and the results are shown in Table 1.
Embodiment 2
Weigh 3000 grams of polypropylene, 6 grams of antioxidant 1010s, 3 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of sorbitol anhydride lists
Stearate, 1.5 gram of two tertiary amyl peroxide, 30 grams of contents of ethylene molar ratios are the poly-methyl of ethenyl blocking of 96%
Silicone oil, 4 grams of styrene, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Embodiment 3
Weighing 3000 grams of polypropylene, 5 grams of antioxidant 1076s, 2 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of monostearates are sweet
Grease, 1.5 grams of benzoyl peroxides, 60 grams of contents of ethylene molar ratios are the poly-methyl-silicone oil of ethenyl blocking and 4 of 96%
Gram styrene, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Embodiment 4
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of erucyl amides, 1.8 grams of monostearates
Glyceride, 1.5 grams of di-t-butyl peroxides, 30 grams of contents of ethylene molar ratios are the poly-methyl-silicone oil of ethenyl blocking of 96%
With 8 grams of styrene, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Embodiment 5
Weighing 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 6 grams of calcium stearates, 1.8 grams of monostearates are sweet
Grease, 2 grams of dicumyl peroxides, 15 grams of contents of ethylene molar ratios are the ethenyl blocking methyl phenyl silicone oil and 20 of 90%
Gram cyclopentadiene, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Embodiment 6
Weighing 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 5 grams of monostearates are sweet
Grease, 3 gram 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane, 30 grams of contents of ethylene molar ratios are the second of 96%
Thiazolinyl blocks poly-methyl-silicone oil and 4 grams of styrene, in stirrer for mixing 20min to uniformly.The same embodiment of extruding pelletization process
1。
Embodiment 7
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of single behenic acids
Glyceride, 1.5 gram 2,5-dimethyl-2,5-di-tert-butyl peroxide alkynes, in stirrer for mixing 20min to uniformly.Will
Mixture adds in double screw extruder, and screw speed is 60 r/min, and rate of feeding is 4.8 kg/h, the revolution of extruder
It is set as 15 revs/min.Extruder is divided into four thermals treatment zone, and wherein a Heating Zone Temperature is set as 165 DEG C, two Heating Zone Temperature
Being set as 180 DEG C, three Heating Zone Temperature are set as 190 DEG C, and four Heating Zone Temperature are set as 190 DEG C.60 grams of contents of ethylene rub
Your ratio be 96% the poly-methyl-silicone oil of ethenyl blocking and 10 grams of styrene stir, enter from the 3rd thermal treatment zone charging aperture
Material, extruding pelletization, obtain high bath strength acrylic resin.
Comparative example 1
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of monostearates
Glyceride, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Comparative example 2
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of monostearates
Glyceride, 1.5 grams of benzoyl peroxides, 60 grams of contents of ethylene molar ratios are the poly-methyl-silicone oil of ethenyl blocking of 96%,
In stirrer for mixing 20min to uniformly.Extruding pelletization process is with embodiment 1.
Comparative example 3
Weigh 3000 grams of polypropylene, 3 grams of antioxidant 1010s, 1.5 grams of irgasfos 168s, 1.5 grams of calcium stearates, 1.8 grams of monostearates
Glyceride, 1.5 grams of benzoyl peroxides, 6 grams of styrene, in stirrer for mixing 20min to uniformly.Extruding pelletization process is with real
Execute example 1.
The present invention can summarize with other the concrete form without prejudice to the spirit or essential characteristics of the present invention.The present invention's
Above-described embodiment all can only be considered the description of the invention rather than restriction, therefore suitable with claims of the present invention
Implication and scope in any change, be all considered as being included within the scope of the claims.
Claims (10)
1. a long-chain branch high fused mass strength polypropylene resin, it is characterised in that main following mass fraction raw material preparation and
Become:
Ethylene propylene copolymer polypropylene 100 parts
Antioxidant 0.10～2 parts
Lubricant 0.05～1 part
Antistatic additive 0.05～1 part
Peroxide initiator 0.01～3 parts
First grafted monomers 0.01～5 parts
Second grafted monomers 0.01～5 parts；
Described first grafted monomers is vinyl-terminated silicone oil, described second grafted monomers be cycloolefin, styrene or both
Combination.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described ethylene, propylene is altogether
Poly-polyacrylic melt flow rate (MFR) 8～10g/10min, ethylene contents is 7～10%.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described antioxidant is for being obstructed
Phenolic antioxidant and the combination of phosphite ester kind antioxidant, wherein, Hinered phenols antioxidant and phosphite antioxidant it
Between mass ratio be 1:1 3:1.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 3, it is characterised in that described Hinered phenols resists
Oxygen agent is 2,6 di tert butyl 4 methyl phenol, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester
With a kind of or both combinations above in β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid octadecyl ester；Described Asia
Phosphate-based antioxidants is trisnonyl phenyl phosphite or tricresyl phosphite (2,4-di-tert-butyl-phenyl) ester.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described lubricant is stearic
One or more combination in acid calcium, erucyl amide and behenic acid amide.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described antistatic additive is
Polyol fatty acid ester compounds；Described polyol fatty acid ester compounds is sorbitan monostearate, single tristearin
One or more combination in acid glyceride and single Glyceryl Behenate.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described peroxide draws
Sending out agent is 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane, di-t-butyl peroxide, cumyl peroxide, peroxide
Change in benzoyl, 2,5-dimethyl-2,5-di-tert-butyl peroxide alkynes and two tertiary amyl peroxide one or both
Above combination.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described ethenyl blocking silicon
Oil for contents of ethylene be more than 80% the poly-methyl-silicone oil of ethenyl blocking or ethenyl blocking methyl phenyl silicone oil or both
Combination.
Long-chain branch high fused mass strength polypropylene resin the most according to claim 1, it is characterised in that described cycloolefin is ring penta
Diene.
10. the preparation method of the long-chain branch high fused mass strength polypropylene resin described in any one of claim 1-9, its feature exists
In, by ethylene propylene copolymer polypropylene, antioxidant, lubricant, antistatic additive, peroxide initiator, the first grafted monomers and
After second grafted monomers mix homogeneously, through double screw extruder extruding pelletization, obtain long-chain branch high fused mass strength polypropylene pellet；
Or, ethylene propylene copolymer polypropylene, antioxidant, lubricant, antistatic additive and peroxide initiator are the most mixed
In clutch after mix homogeneously, adding in double screw extruder, described first grafted monomers and the second grafted monomers are from extruder
Second, third or the throat-fed of the 4th feeding section, melt extrude pelletize, obtain long-chain branch high fused mass strength polypropylene grain
Material.
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