CN111518336A - Controllable rheological polypropylene material and preparation method and application thereof - Google Patents
Controllable rheological polypropylene material and preparation method and application thereof Download PDFInfo
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 117
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 116
- -1 polypropylene Polymers 0.000 title claims abstract description 90
- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 150000002978 peroxides Chemical class 0.000 claims abstract description 45
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 239000011358 absorbing material Substances 0.000 claims abstract description 4
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 23
- 238000000518 rheometry Methods 0.000 claims description 16
- 239000002480 mineral oil Substances 0.000 claims description 14
- 235000010446 mineral oil Nutrition 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000155 melt Substances 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 8
- 229920005629 polypropylene homopolymer Polymers 0.000 claims description 6
- MOVRNJGDXREIBM-UHFFFAOYSA-N aid-1 Chemical compound O=C1NC(=O)C(C)=CN1C1OC(COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)CO)C(O)C1 MOVRNJGDXREIBM-UHFFFAOYSA-N 0.000 claims description 5
- 239000000314 lubricant Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 229940037312 stearamide Drugs 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- 239000012933 diacyl peroxide Substances 0.000 claims description 2
- 239000012774 insulation material Substances 0.000 claims description 2
- MMCOUVMKNAHQOY-UHFFFAOYSA-L oxido carbonate Chemical compound [O-]OC([O-])=O MMCOUVMKNAHQOY-UHFFFAOYSA-L 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 5
- 239000004033 plastic Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 229920001002 functional polymer Polymers 0.000 abstract description 2
- 239000011810 insulating material Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002144 chemical decomposition reaction Methods 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000012968 metallocene catalyst Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000007363 regulatory process Effects 0.000 description 2
- 102220040412 rs587778307 Human genes 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- DDNCQMVWWZOMLN-IRLDBZIGSA-N Vinpocetine Chemical compound C1=CC=C2C(CCN3CCC4)=C5[C@@H]3[C@]4(CC)C=C(C(=O)OCC)N5C2=C1 DDNCQMVWWZOMLN-IRLDBZIGSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 239000012969 di-tertiary-butyl peroxide Substances 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 150000001451 organic peroxides Chemical group 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005633 polypropylene homopolymer resin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229960000744 vinpocetine Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- 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
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
-
- 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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
-
- 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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- 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
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention belongs to the technical field of functional polymer materials, and discloses a controllable rheological polypropylene material and a preparation method and application thereof. The controllable rheological polypropylene material comprises the following components in parts by weight: 1-10 parts of peroxide master batch, 0-1 part of processing aid and 90-99 parts of homopolymerized polypropylene. Wherein the peroxide master batch comprises the following components in parts by weight: 90-99 parts of homopolymerized polypropylene powder, 1-10 parts of initiator and 0-1 part of processing aid. The invention solves the dispersion of peroxide in matrix resin and the contradiction between low-temperature stable processing of peroxide and polypropylene melt temperature through a two-step method. Meanwhile, the problem of complete reaction of the peroxide is solved by a two-step method. The controllable rheological polypropylene plastic particles have controllable rheological property, narrow molecular weight distribution and low smell, and have diversified application prospects in the fields of heat-insulating materials, medical sanitary materials, filtering materials and automobile sound-absorbing materials.
Description
Technical Field
The invention belongs to the technical field of functional polymer materials, and particularly relates to a controllable rheological polypropylene material and a preparation method and application thereof.
Background
The high flow polypropylene (PP) generally refers to polypropylene with Melt Flow Rate (MFR) of more than or equal to 20g/10min, and is a novel special PP resin developed since the 21 st century. The resin not only has higher melt fluidity, but also has excellent rigidity and toughness balance, is often applied to large thin-wall injection molding products, such as household electrical appliances, automobile parts, industrial parts, food and medical packaging and the like, and greatly accelerates the development of large thin-wall manufacturing industries of automobiles, household products, packaging and the like. The ultra-high fluidity polypropylene resin is polypropylene with Melt Flow Rate (MFR) of more than or equal to 400g/10 min.
The high flow impact polypropylene is produced in three ways: the first is hydrogen regulation method, the second is controllable rheological method, and the third is metallocene catalyst method. The hydrogen regulating process has great amount of hydrogen added to the polymerization reaction to terminate the reaction, so that the molecular weight of polypropylene is reduced, the flowability of the product is raised, and the polypropylene product produced through the hydrogen regulating process has wide molecular weight distribution and is favorable to forming. Meanwhile, because no peroxide exists in the production process, the problem of odor does not exist in the plastic products. Meanwhile, the whiteness of the product is greatly improved and can be kept for a long time. The melt flow rate can be kept relatively stable in the processing process needing multiple times of heating, and the control of the quality of downstream products is facilitated. The hydrogen regulation method has the disadvantages that the polymerization technical requirement is high, the original catalyst system needs to be improved, the production cost of the product is increased, more importantly, the range of regulating the melt flow rate of the polypropylene by the hydrogen regulation method is limited, the melt flow rate can be regulated within the range of 20-40g/10min, and the application field of the hydrogen regulation method is severely limited. The metallocene catalyst method has extremely high technical requirements on the catalyst, the production process is complex, the energy cost of the produced product is extremely high, and the method is rarely applied at home at present. The controllable rheological process, also called chemical degradation process, is to add peroxide into the pelletizing unit of the polymerization apparatus to break the chain of polypropylene and thus regulate the melt flow rate of the final product. The chemical degradation method has the advantages of early development and application, relatively simple and flexible operation and low realization cost. Thus degradation processes are widely used in the production of high flow polypropylene products. The company DOW chemical obtains ultra high flow and balanced stiffness and toughness products with MFR of 70 and 100g/min by chemical degradation of a copolymer produced in a reactor and having MFR of 35 g/min. The use of a small amount of a degradation agent minimizes the reduction in toughness. However, peroxide degradation products, especially t-butyl alcohol, degrade and if the degradation is not sufficient, the resulting plastic particles have an unpleasant odor.
In addition, the grant number CN101942146B discloses a controlled-rheology high-gloss polypropylene resin, which is composed of the following components: 100 portions of homopolymerized polypropylene is taken as a base material, the number average molecular weight of the homopolymerized polypropylene is 61235-65210, 0.1-0.25 portion of processing aid, 0.15-0.2 portion of nucleating agent, 0-1.5 portions of hardness regulator, 0.05-0.1 portion of gloss regulator and 1-12 portions of peroxide master batch are added, the peroxide master batch is formed by mixing 100 portions of homopolymerized polypropylene and 0.1-0.65 portion of peroxide, and the rheological property of the resin can be changed by adjusting the amount of the added peroxide master batch. The controllable rheological high-gloss polypropylene resin has excellent heat resistance (the heat distortion temperature is more than or equal to 110 ℃) and higher rigidity (the flexural modulus is more than or equal to 1800 MPa). Because of adopting the controllable rheological technology, the melt flow rate of the material can be flexibly adjusted, and the material has excellent molding processing performance, heat resistance and mechanical property. But the melt flow rate of the special material prepared by the method can be from 7 to 100g/10 min. The range of application thereof is limited.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a controllable rheological polypropylene material;
the invention also aims to provide a preparation method of the controllable rheological polypropylene material.
It is a further object of the present invention to provide the use of the above controlled rheology polypropylene material.
The purpose of the invention is realized by the following scheme:
the controllable rheological polypropylene material comprises the following components in parts by weight:
1-50 parts of peroxide master batch
49-99 parts of homopolymerized polypropylene
10-1 parts of a processing aid.
Preferably, the controlled rheology polypropylene material comprises the following components in parts by weight:
3-50 parts of peroxide master batch
49-96.5 parts of homopolymerized polypropylene
10.5-1 parts of processing aid.
In the controllable rheological polypropylene material, the homopolymerized polypropylene refers to at least one of homopolymerized polypropylene granules with the melt mass flow rate of 1-40 g/10min (test conditions: 230 ℃ and 2.16 KG). Preferably at least one of Dalianxitai PP T30, Mediterranean Shell HP502N, Maoming petrochemical PP Z30S, and more preferably Maoming petrochemical PP Z30S;
in the controlled-rheology polypropylene material, the processing aid 1 is at least one of stearamide lubricants (such as EBS ethylene bis stearamide), silicone oil and white mineral oil, and the white mineral oil is preferred.
In the controllable rheological polypropylene material, the peroxide master batch comprises the following components in parts by weight:
90-99 parts of homopolymerized polypropylene powder
1-10 parts of initiator
And 20-1 part of a processing aid.
In the peroxide master batch, the homopolymerized polypropylene powder refers to at least one of homopolymerized polypropylene powder with the melt mass flow rate of 1-40 g/10min (test conditions: 230 ℃ and 2.16KG), preferably at least one of Dalixiao TaiPP T30S powder and Zhejiang hongji PPH225 powder, and more preferably Zhejiang hongji PPH225 powder.
In the peroxide master batch, the initiator is organic peroxide, specifically hydroperoxide (ROOH), dialkyl peroxide (ROOR '), diacyl peroxide (RCOOCR'), peroxyester (RCOOOR '), peroxycarbonate (ROOOOOCOR') and ketone peroxide [ R ]2C(OOH)2]Etc., preferably TX101 of akkusu, and exuberant of jiangsu
At least one of DTBPs, more preferably aksu TX 101.
In the peroxide master batch, the processing aid 2 is at least one of stearamide lubricants (such as EBS ethylene bis stearamide), silicone oil and white mineral oil, and is preferably Ethylene Bis Stearamide (EBS).
The preparation method of the controlled-rheology polypropylene material comprises the following steps:
a. adding the homo-polypropylene powder, the initiator and the processing aid 2 into a low-speed mixer according to a certain proportion, mixing to obtain a premix, and putting the premix into a single-screw extruder for extrusion granulation to obtain peroxide master batches;
b. and adding the peroxide master batch, the homo-polypropylene and the processing aid 1 into a low-speed mixer according to a proportion, mixing to obtain a premix, and then putting the premix into a double-screw extruder for extrusion granulation to obtain the controllable rheological polypropylene material.
In the step a, the temperature of a single-screw extruder barrel is controlled to be between 90 and 140 ℃, the rotating speed of a main machine is 100 plus 300r/min, and the rotating speed of feeding is 100 plus 300 r/min;
in the step b, the temperature of the double-screw extruder barrel is controlled to be 180-230 ℃, the rotating speed of the main machine is 500-800 r/min, and the feeding rotating speed is 200-800 r/min.
The mixing in the low-speed mixer in the step a and the step b refers to mixing for 2-10min at the rotating speed of 0-60r/min and then mixing for 1-5min at the rotating speed of 60-120 r/min.
The controllable rheological polypropylene plastic particles have extremely high fluidity, narrow molecular weight distribution and low smell, and have diversified application prospects in the fields of heat-insulating materials, medical sanitary materials, filtering materials, automobile sound-absorbing materials and other markets.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention discloses a controllable rheological polypropylene material and a preparation method and application thereof, which solve the problem of dispersion of peroxide in matrix resin on one hand and the problem of contradiction between low-temperature stable processing of the peroxide and the temperature of a polypropylene melt on the other hand through a two-step method. Meanwhile, the problem of complete reaction of the peroxide is solved by a two-step method. The melt flow rate of the controllable rheological polypropylene material prepared by the method is adjustable within the range of 40-3000g/10min, so that the application range and the field of the controllable rheological polypropylene material are greatly expanded. The controllable rheological polypropylene plastic particles prepared by the method have extremely high fluidity, narrow molecular weight distribution and low odor, and have diversified application prospects in the fields of thermal insulation materials, medical sanitary materials, filtering materials, automobile sound-absorbing materials and other markets.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the examples, the low speed mixer used to prepare the controlled rheology polypropylene material was SHR-100A manufactured by Kodak machines, Inc., of hong Kong, Jiangsu;
in the examples, the twin screw extruder used to prepare the controlled rheology polypropylene material was SHJ-30 manufactured by Nanjing Ruiya Polymer Equipment Ltd;
in the embodiment, the injection molding machine used for testing the sample strip of the controllable rheological polypropylene material is B-920 produced by Zhejiang Haitian injection molding machine Co., Ltd;
in the examples, differential scanning calorimetry: mertler, switzerland; melting and crystallization were analyzed by DSC in nitrogen (N)2Flow 50mL/min), heating about 5mg of sample to 210 ℃ at a heating rate of 20 ℃/min, keeping the temperature for 5min, and then cooling to 30 ℃ at a cooling rate of 20 ℃/min;
in the examples, vicat softening point/heat distortion temperature tester: vinpocetine intelligent instruments and equipment limited. The Vicat softening temperature is tested by adopting the GB/T1633 standard, the weight is 1000 g, and the heating rate is 12 ℃/6 min.
In the examples, melt index meter: ATSFAAR, Italy; the test is carried out by adopting the GB/T3682-2000 standard, the test temperature is 230 ℃, and the weight mass is 2.16 kg.
In the examples, gel permeation chromatography: GPC2000 WATER corporation; o-dichlorobenzene is used as a solvent, and the sample is injected at the speed of 1.0mL/min at the temperature of 135 ℃, and polystyrene is used as a standard sample.
The compositions prepared in each example were injection molded in standard sizes into test bars, and the properties in each example were measured using the following standards, as shown in Table 1.
TABLE 1 test standards
1. Melt index test conditions: 230 ℃/2.16KG
2. Thermal deformation temperature test conditions: 4mm/0.45MPa
In the following examples, homopolypropylene resin powders were respectively selected from Dalixi TaiPP T30S powder and Zhejiang hongji PPH225 powder; the homopolymerized polypropylene granules respectively adopt Dalixi Tai PP T30, Zhonghai brand HP502N, Mount petrochemical PPZ30S and the like; initiator is Acksu TX101, Jiangsu is vigorous
DTBP; the processing aid is a general commodity in the current market.
Example 1
(1) The peroxide master batch (PPMB1) comprises the following components in parts by weight:
89 parts of PP 225 powder
TX 10110 parts
1 part of No. 70 white mineral oil
(2) The preparation method comprises the following steps: adding the components in the specified proportion into a low-speed mixer, mixing for 2-10min at the rotating speed of 0-30r/min, mixing for 1-5min at the rotating speed of 30-60r/min to obtain a premix, putting the premix into a single-screw extruder for extrusion and granulation, controlling the temperature of the single-screw extruder barrel at 10 sections, controlling the temperature at 90-140 ℃, controlling the rotating speed of a main machine at 300r/min and the feeding rotating speed at 100 + 300r/min, and performing extrusion and granulation to prepare the peroxide master batch. The measured data are shown in Table 2.
Example 2
(1) The peroxide master batch (PPMB2) comprises the following components in parts by weight:
94 portions of PP 225 powder
TX 1015 parts
1 part of No. 70 white mineral oil
The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Example 3
(1) The peroxide master batch (PPMB3) comprises the following components in parts by weight:
98 portions of PP 225 powder
TX 1011 parts
1 part of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Example 4
(1) The peroxide master batch (PPMB4) comprises the following components in parts by weight:
99 parts of PP 225 powder
TX 1011 parts
0 portion of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Example 5
(1) The peroxide master batch (PPMB5) comprises the following components in parts by weight:
95 parts of PP 225 powder
TX 1015 parts
0 portion of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Example 6
(1) The peroxide master batch (PPMB6) comprises the following components in parts by weight:
94.5 portions of PP 225 powder
TX 1015 parts
0.5 portion of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Comparative example 1
(1) The peroxide master batch (PPMB7) comprises the following components in parts by weight:
HP502N 94.5.5 parts
TX 1015 parts
0.5 portion of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Comparative example 2
(1) The peroxide master batch (PPMB8) comprises the following components in parts by weight:
PP Z30S 94.5.5 parts
TX 1015 parts
0.5 portion of No. 70 white mineral oil
(2) The preparation process is the same as that of example 1, and the measured data are shown in Table 2.
Example 7
The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 15 parts
PP Z30S 94 part
EBS 1 part
(2) The PPMB1 master batch and the components are added into a low-speed mixer according to the proportion and mixed for 2-10min at the rotating speed of 0-60r/min, and then mixed for 1-5min at the rotating speed of 60-120r/min to obtain a premix, the premix is put into a double-screw extruder for extrusion and granulation, the temperature of the double-screw extruder barrel is controlled by 10 sections, the temperature is controlled at 180-230 ℃, the rotating speed of a host machine is controlled at 500-1500r/min, the feeding rotating speed is 200-800r/min, and the controllable rheological polypropylene material is obtained by extrusion and granulation. Adding the particles into an injection molding machine to be processed into a required sample strip, wherein the injection molding conditions are as follows: the temperature of the charging barrel is 220 ℃, the temperature of the die is 60-70 ℃, and the injection pressure is 8 MPa. The measured data are shown in Table 3.
Example 8
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
210 portions of PPMB
PP Z30S 89 parts
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Example 9
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
350 portions of PPMB
PP Z30S 49 part
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Example 10
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 450 parts
PP Z30S 49 part
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Example 11
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
510 portions of PPMB
PP Z30S 89 parts
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Example 12
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
610 portions of PPMB
PP Z30S 89 parts
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Comparative example 3
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 710 parts
PP Z30S 89 parts
EBS 1 part
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 3.
Comparative example 4
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 810 parts
PP Z30S 89 parts
EBS 1 part
(2) The preparation method is the same as example 7, and the measured data are shown in Table 3
Example 13
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 11 parts
PP Z30S 98.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 14
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 13 parts
PP Z30S 96.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 15
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
PPMB 15 parts
PP Z30S 94.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 16
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
110 portions of PPMB
PP Z30S 92.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 17
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
115 parts of PPMB
84.5 parts of PP Z30S 84.5
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 18
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
120 portions of PPMB
PP Z30S 79.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 19
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
130 portions of PPMB
PP Z30S 69.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
Example 20
(1) The controllable rheological polypropylene material comprises the following components in parts by weight:
150 portions of PPMB
PP Z30S 49.5.5 parts
0.5 portion of EBS
(2) The preparation method is the same as that of example 7, and the measured data are shown in Table 4.
TABLE 2 physicochemical Properties data for the tests of examples 1-6 and comparative examples 1-2
TABLE 3 physicochemical Properties data for the tests of examples 7-12 and comparative examples 3-4
TABLE 4 data sheet of physicochemical properties of tests of examples 13 to 20
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The controllable rheological polypropylene material is characterized by comprising the following components in parts by weight:
1-50 parts of peroxide master batch
49-99 parts of homopolymerized polypropylene
10-1 parts of a processing aid.
2. The controlled rheology polypropylene material according to claim 1, characterized by comprising the following components in parts by weight:
3-50 parts of peroxide master batch
49-96.5 parts of homopolymerized polypropylene
10.5-1 parts of processing aid.
3. A controlled rheology polypropylene material according to claim 1 or 2, characterized in that:
in the controllable rheological polypropylene material, the homopolymerized polypropylene refers to at least one of homopolymerized polypropylene granules with the melt mass flow rate of 1-40 g/10 min; the processing aid 1 is at least one of stearamide lubricants, silicone oil and white mineral oil.
4. A controlled rheology polypropylene material according to claim 3, characterized in that:
in the controllable rheological polypropylene material, the homo-polypropylene is at least one of Dalixitai PP T30, Zhonghai Shell HP502N and Michelson PP Z30S; the processing aid 1 is white mineral oil.
5. A controlled rheology polypropylene material according to claim 3, characterized in that:
the peroxide master batch comprises the following components in parts by weight:
90-99 parts of homopolymerized polypropylene powder
1-10 parts of initiator
And 20-1 part of a processing aid.
6. A controlled rheology polypropylene material according to claim 5, characterized in that:
in the peroxide master batch, the homopolymerized polypropylene powder refers to at least one of homopolymerized polypropylene powder with the melt mass flow rate of 1-40 g/10 min;
in the peroxide master batch, the initiator is at least one of hydroperoxide, dialkyl peroxide, diacyl peroxide, peroxyester, peroxycarbonate and ketone peroxide;
in the peroxide master batch, the processing aid 2 is at least one of stearamide lubricant, silicone oil and white mineral oil.
7. A controlled rheology polypropylene material according to claim 5, characterized in that:
in the peroxide master batch, the homo-polypropylene powder refers to Zhejiang hongji PPH225 powder;
in the peroxide master batch, the initiator is Acksu TX 101;
in the peroxide master batch, the processing aid 2 is ethylene bis stearamide.
8. A process for the preparation of a controlled rheology polypropylene material according to any of claims 1 to 7, characterized by comprising the steps of:
a. adding the homo-polypropylene powder, the initiator and the processing aid 2 into a low-speed mixer according to a certain proportion, mixing to obtain a premix, and putting the premix into a single-screw extruder for extrusion granulation to obtain peroxide master batches;
b. and adding the peroxide master batch, the homo-polypropylene and the processing aid 1 into a low-speed mixer according to a proportion, mixing to obtain a premix, and then putting the premix into a double-screw extruder for extrusion granulation to obtain the controllable rheological polypropylene material.
9. The method of preparing a controlled rheology polypropylene material according to claim 8, characterised in that:
in the step a, the temperature of a single-screw extruder barrel is controlled to be between 90 and 140 ℃, the rotating speed of a main machine is 100 plus 300r/min, and the rotating speed of feeding is 100 plus 300 r/min;
in the step b, the temperature of the double-screw extruder barrel is controlled to be 180-230 ℃, the rotating speed of the main machine is 500-;
the mixing in the low-speed mixer in the step a and the step b refers to mixing for 2-10min at the rotating speed of 0-60r/min and then mixing for 1-5min at the rotating speed of 60-120 r/min.
10. Use of the controlled rheology polypropylene material according to any of claims 1 to 7 for the preparation of thermal insulation materials, medical hygiene materials, filter materials, automotive sound absorbing materials.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143115A (en) * | 2020-09-18 | 2020-12-29 | 会通新材料(上海)有限公司 | Preparation method of flame-retardant polypropylene material |
| CN114181453A (en) * | 2021-11-04 | 2022-03-15 | 金发科技股份有限公司 | Low-friction-coefficient low-atomization polypropylene material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103571039A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工股份有限公司 | High-melt index polypropylene composition and preparation method thereof |
| WO2014069911A1 (en) * | 2012-11-05 | 2014-05-08 | 주식회사 만텍 | Technology for producing peroxide masterbatches, and method for reforming polypropylene using same |
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2020
- 2020-05-28 CN CN202010467560.3A patent/CN111518336A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571039A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工股份有限公司 | High-melt index polypropylene composition and preparation method thereof |
| WO2014069911A1 (en) * | 2012-11-05 | 2014-05-08 | 주식회사 만텍 | Technology for producing peroxide masterbatches, and method for reforming polypropylene using same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143115A (en) * | 2020-09-18 | 2020-12-29 | 会通新材料(上海)有限公司 | Preparation method of flame-retardant polypropylene material |
| CN114181453A (en) * | 2021-11-04 | 2022-03-15 | 金发科技股份有限公司 | Low-friction-coefficient low-atomization polypropylene material and preparation method and application thereof |
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