CN109593276A - A kind of damage resistant high-impact atactic copolymerized polypropene and preparation method thereof - Google Patents
A kind of damage resistant high-impact atactic copolymerized polypropene and preparation method thereof Download PDFInfo
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- CN109593276A CN109593276A CN201710917787.1A CN201710917787A CN109593276A CN 109593276 A CN109593276 A CN 109593276A CN 201710917787 A CN201710917787 A CN 201710917787A CN 109593276 A CN109593276 A CN 109593276A
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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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- 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
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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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
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of damage resistant high-impact atactic copolymerized polypropenes and preparation method thereof.Damage resistant high-impact atactic copolymerized polypropene resin, its raw material components includes: 100 parts of copolymer polypropylene base-materials, 0-0.1 parts of antioxidant, 0-0.1 parts of halogen-absorbers, 1-3 parts of organically-modified silicone, 5-15 parts of toughener and 1-10 parts of peroxide master batches, the number are parts by weight.Transparent polypropylene PP Pipe Compound of the invention has scratch resistant performance outstanding and toughness, can flexibly adjust the melt flow rate (MFR) of material, obtain different processing characteristics.
Description
Technical field
The present invention relates to a kind of damage resistant high-impact atactic copolymerized polypropenes and preparation method thereof, belong to polypropylene technology neck
Domain.
Background technique
In recent years, continuing the deeply increasingly raising of the people's material and cultural life level, domestic city with reform and opening-up
Field grows at top speed to the demand of high-transparency polypropylene PP Pipe Compound, and application field is also more and more extensive, while also special to polypropylene
Erosion-resisting characteristics, transparency and the scratch resistant performance of materials propose increasingly higher demands, especially in food containers, household electric
The technical fields such as device, thin-walled and large size or complex parts injection molding production.
Although there is the report of the research and development of many atactic copolymerized polypropene resin materials in the country at present, it is essentially confined to
All there is punching such as M800E, M1600E that R370Y, the oil of SPC of SK company, South Korea are developed in the polyacrylic exploitation of normal transparent
The weakness that hit intensity is low, scratch resistant performance is poor seriously constrains product and promotes and applies in the market.The country yet there are no scratch-resistant at present
Hurt the related patents report of high impact resistance polypropylene resin material.
Summary of the invention
It is lacked to solve in the prior art that atactic copolymerized polypropene resin material impact strength is low, scratch resistant performance is poor etc.
It falls into, the present invention provides a kind of damage resistant high-impact atactic copolymerized polypropene and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of damage resistant high-impact atactic copolymerized polypropene resin, raw material components include: 100 parts of copolymer polypropylene bases
Material, 0-0.1 parts of antioxidant, 0-0.1 parts of halogen-absorbers, 1-3 parts of organically-modified silicone, 5-15 parts of toughener and 1-10 parts of peroxides
Compound masterbatch, the number are parts by weight.
Since melt flow rate (MFR) of the different products injection molding for resin requires difference, the present invention uses controllable rheology skill
Art is added ethylene-alpha-octylene copolymer elastomer and organically-modified silicone compound auxiliary, is opened on the basis of Amoco gas phase process
Issue the damage resistant high impact resistance polypropylene resin of function admirable.Due to using controllable rheology technology, material can be flexibly adjusted
Melt flow rate (MFR), obtain different processing characteristics.Material has excellent performance, suitable for different wall thickness injection-molded item
Production.
In order to promote the synergistic effect between each component, antioxidant is β-(4- hydroxyl -3,5- di-tert-butyl-phenyl) propionic acid
Positive at least one of octadecanol ester or phosphorous acid three (2.4- di-tert-butyl-phenyl) ester.
In order to promote the synergistic effect between each component, to further increase the impact strength and scratch resistance of material
Can, halogen-absorber is calcium stearate；Toughener is ethylene-alpha-octylene copolymer elastomer.
In order to promote the synergistic effect between each component, to further increase the impact strength and scratch resistance of material
Can, the melt flow rate (MFR) of copolymer polypropylene base-material is 0.1-400g/10min, preferably 1-80g/10min, and measuring condition is
190 DEG C, 21.6kg；Molecular weight distribution is not more than 4, preferably 1.8-3.5, more preferably 2.1-2.7.
In order to further increase the impact strength and scratch resistant performance of material, peroxide master batch will be the preparation method is as follows: will
100 parts by weight homopolypropylene and 0.65 parts by weight di-tert-butyl peroxide stir evenly, and are with double screw extruder extrusion
?.
Copolymer polypropylene base-material is formed by propylene monomer, fluoride monomers, and polymerization process is catalyzed using solid polyolefin
Agent；Polymerization pressure is that atmosphere is depressed into 100kg/cm2, and preferably atmosphere is depressed into 60kg/cm2；
The each component of solid polyolefin hydrocarbon catalyst mixes in polymer reactor, or adds in reactor after premix；
If it is premixing, being pre-mixed temperature is -50 DEG C -160 DEG C, and preferable is -20-110 DEG C, and time of contact is 1-1500 minutes,
Preferable is 4-500 minutes；
Polymerization is carried out using liquid polymerization method or gas phase polymerization process；
In liquid phase polymerization, use unreactive hydrocarbons solvent or propylene itself as solvent；
In suspension polymerisation, polymerization temperature is -50-150 DEG C, preferably 10-90 DEG C；In solution polymerization, temperature is
0-250 DEG C, preferably 30-180 DEG C；During gas phase polymerization, temperature is 0-130 DEG C, preferably 20-90 DEG C.
Polymerization reaction can in batches, it is semicontinuous or be carried out continuously.Polymerization can also be in two steps or more under the conditions of differential responses
Step carries out.
The preparation method of above-mentioned damage resistant high-impact atactic copolymerized polypropene resin, by copolymer polypropylene base-material, antioxidant,
Halogen-absorber, organically-modified silicone and toughener are uniformly mixed, and are then added in the main spout of double screw extruder, through double
Screw extruder squeeze out, pelletizing to get；When double screw extruder squeezes out, it is added from the auxiliary spout of double screw extruder
Peroxide master batch, controlling main spout and assisting the feeding mass-velocity ratio of spout is 100:1-100:10.
In order to further increase the comprehensive performance of material, each area's temperature setting of double screw extruder are as follows: Z1:185-195
DEG C, Z2:205-215 DEG C, Z3:210-220 DEG C, Z4:215-225 DEG C, Z5:215-225 DEG C, Z6:210-220 DEG C, head: 205-
215 DEG C, double-screw extruder screw revolving speed is 310rpm.
Z1-Z6 respectively represents first segment to the 6th section.
The unmentioned technology of the present invention is referring to the prior art.
Damage resistant high impact resistance polypropylene resin of the present invention has scratch resistant performance outstanding (Δ L < 2) and very high toughness
(room temperature impact strength >=10kJ/m2)；The melt flow rate (MFR) that material can flexibly be adjusted, obtains different processing characteristics；
Material has excellent moulding processability, shock resistance and optical property, can shorten the processing and forming period of product, mention
The apparent property of high product, the production suitable for different wall thickness injection-molded item.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
In following embodiments, the room temperature (23 DEG C) and low temperature (- 20 DEG C) simply supported beam notch impact strength of material measure reference
GB/T 1043.1-2008 carries out (unit kJ/m2)；The tensile property measurement of material is carried out referring to GB/T 1040.2-2006
(unit MPa)；The heat distortion temperature measurement of material carries out (unit is DEG C) referring to GB/T 1634.2-2004.Material it is scratch-resistant
Hurt performance measurement to carry out referring to GM10640；Glossiness is carried out referring to GB/T 8807-1988；Scratch resistant is referring to Shanghai Volkswagen
PV3952 test.
Embodiment 1
By 100 parts by weight homopolypropylene (F401, the production of Yangtze petrochemical industry Co., Ltd), the tertiary fourth of 0.65 parts by weight two
Base peroxide (DTBP, Tianjin Lisheng Chemical Co., Ltd.'s production), which is placed in high-speed mixer, to stir evenly, and is squeezed with twin-screw
Machine (TE35 type, subfamily skill Development Co., Ltd, Nanjing section) extruding pelletization at a temperature of being not higher than 190 DEG C is female at peroxide out
Expect spare.
By the atactic copolymerized polypropene (self-control) of 100 parts by weight, the phenolic antioxidant β-of 0.10 parts by weight (hydroxyl -3 4-,
5- di-tert-butyl-phenyl) and propionic acid n-octadecyl alcohol ester (article number: 1076, Ciba), the phosphorous acid three of 0.10 parts by weight
(2.4- di-tert-butyl-phenyl) ester, (the limited public affairs of magnificent industry are inspired confidence in high-purity calcium stearate, Shanghai to the halogen-absorber of 0.10 parts by weight
Department), the organically-modified silicone (BASF IRGASURF SR100) of 2 parts by weight and the ethylene-alpha-octylene of 5 parts by weight are copolymerized elasticity
Body (Engage 8130, Dow Chemical production), which is placed in high-speed mixer, to stir evenly, and it is spare to obtain base-material.By gained
Base-material and peroxide master batch be respectively placed in the master of double screw extruder (TE35 type, subfamily skill Development Co., Ltd, Nanjing section)
In material and auxiliary material loading hopper, the feed screw revolving speed of major ingredient and auxiliary material is adjusted, control main spout and assists the feeding of spout
Mass-velocity ratio is 100:1.Each area's temperature of double screw extruder is set are as follows: Z1:190 DEG C, Z2:210 DEG C, Z3:215 DEG C, Z4:
220 DEG C, Z5:220 DEG C, Z6:215 DEG C, head: 210 DEG C.Twin-screw extrusion revolving speed setting are as follows: 310rpm.Last extrudate is through water
Air-dried pelletizing, obtained damage resistant high impact resistance polypropylene composition are denoted as NPO-1 after cold.Its performance test results is shown in Table 1.
Atactic copolymerized polypropene specific the preparation method comprises the following steps:
Major catalyst (TK216), co-catalyst (triethyl aluminum), external electron donor (isobutyl triethoxy silane) [its
Middle TK216 flow is 3.5g/h, triethyl aluminum flow is 5.5g/h, isobutyl triethoxy silane flow is 2.5g/h] through 10
DEG C, prepolymerization reactor is entered after 15min pre-contact, prepolymerization reaction carries out under propylene liquid-phase bulk environment, 15 DEG C of progress 3min,
Enter the first gas-phase polymerization reactor by pre-polymerized catalyst, ethylene, propylene ratio is 0.035 (molar ratio), and reaction temperature is
65.2~74.4 DEG C, reaction pressure is 3.0~4.0MPa, and residence time 0.5h, it is anti-that reaction product enters the second gas-phase polymerization
Device is answered, ethylene, propylene ratio is 0.025 (molar ratio), and reaction temperature is 66.7~73.0 DEG C, and reaction pressure is 3.0~4.0MPa,
Residence time is 0.5h, and the polymer come out from gas-phase polymerization reactor heat drying after flash separation and catalyst deactivation obtains
To polymer powders.
Embodiment 2
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of Engage 8130 is changed to 10 parts.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-2.Its performance test results is shown in Table 1.
Embodiment 3
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of organically-modified silicone auxiliary agent is changed to 2.5 parts by weight, controls main spout and assists the feeding of spout
Mass-velocity ratio is 100:5.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-3.Its performance test results is shown in Table 1.
Embodiment 4
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of Engage 8130 is changed to 15 parts, controls main spout and assists the feeding mass-velocity ratio of spout
For 100:5.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-4.Its performance test results is shown in Table 1.
Embodiment 5
It is substantially the same manner as Example 1, but be with the following changes:
Controlling main spout and assisting the feeding mass-velocity ratio of spout is 100:5.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-5.Its performance test results is shown in Table 1.
Embodiment 6
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of organically-modified silicone is changed to 3 parts by weight, controls main spout and assists the feeding quality speed of spout
Rate ratio is 100:10.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-6.Its performance test results is shown in Table 1.
Embodiment 7
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of Engage 8130 is changed to 10 parts, controls main spout and assists the feeding mass-velocity ratio of spout
For 100:10.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-7.Its performance test results is shown in Table 1.
Embodiment 8
It is substantially the same manner as Example 1, but be with the following changes:
The additional amount of organically-modified silicone is changed to 3 parts by weight, and the additional amount of Engage 8130 is changed to 15 parts, and control is main to feed
Material mouth and the feeding mass-velocity ratio of auxiliary spout are 100:10.
It obtains the damage resistant high impact resistance polypropylene composition and is denoted as NPO-8.Its performance test results is shown in Table 1.
Performance test:
By the test of acrylic resin scratch resistant performance and mechanical performance made from embodiment, 1 the results are shown in Table:
As shown in Table 1, acrylic resin made from the method for the present invention has excellent scratch resistance, the transparency
It is high, toughness is good, can commercial scale, be suitable for manufacturing the pp material of different wall thickness anti-impact injection-molded item.
Claims (9)
1. a kind of damage resistant high-impact atactic copolymerized polypropene resin, which is characterized in that its raw material components includes: 100 parts of copolymerization
Polypropylene base-material, 0-0.1 parts of antioxidant, 0-0.1 parts of halogen-absorbers, 1-3 parts of organically-modified silicone, 5-15 parts of toughener and 1-
10 parts of peroxide master batches, the number are parts by weight.
2. damage resistant high-impact atactic copolymerized polypropene resin as described in claim 1, which is characterized in that antioxidant is β-
In (4- hydroxyl -3,5- di-tert-butyl-phenyl) propionic acid n-octadecyl alcohol ester or phosphorous acid three (2.4- di-tert-butyl-phenyl) ester extremely
Few one kind.
3. damage resistant high-impact atactic copolymerized polypropene resin as claimed in claim 1 or 2, which is characterized in that halogen absorbs
Agent is calcium stearate.
4. damage resistant high-impact atactic copolymerized polypropene resin as claimed in claim 1 or 2, which is characterized in that toughener is
Ethylene-alpha-octylene copolymer elastomer.
5. damage resistant high-impact atactic copolymerized polypropene resin as claimed in claim 1 or 2, which is characterized in that copolymerization poly- third
The melt flow rate (MFR) of alkenyl material is 0.1-400g/10min；Molecular weight distribution is not more than 4.
6. damage resistant high-impact atactic copolymerized polypropene resin as claimed in claim 1 or 2, which is characterized in that peroxide
Masterbatch preparation process is as follows: 100 parts by weight homopolypropylene and 0.65 parts by weight di-tert-butyl peroxide being stirred evenly, are used
Double screw extruder squeezes out to obtain the final product.
7. damage resistant high-impact atactic copolymerized polypropene resin as claimed in claim 1 or 2, which is characterized in that copolymerization poly- third
Alkenyl material is formed by propylene monomer, fluoride monomers, and polymerization process uses solid polyolefin hydrocarbon catalyst；Polymerization pressure is atmosphere
It is depressed into 100kg/cm2；
The each component of solid polyolefin hydrocarbon catalyst mixes in polymer reactor, or adds in reactor after premix；If
It is premixing, premixing temperature is -50 DEG C -160 DEG C, and time of contact is 1-1500 minutes；
Polymerization is carried out using liquid polymerization method or gas phase polymerization process；
In liquid phase polymerization, use unreactive hydrocarbons solvent or propylene itself as solvent；
In suspension polymerisation, polymerization temperature is -50-150 DEG C；In solution polymerization, temperature is 0-250 DEG C；It is poly- in vapor phase method
During conjunction, temperature is 0-130 DEG C.
8. the preparation method of the described in any item damage resistant high-impact atactic copolymerized polypropene resins of claim 1-7, feature
It is, copolymer polypropylene base-material, antioxidant, halogen-absorber, organically-modified silicone and toughener is uniformly mixed, are then added
In the main spout of double screw extruder, through double screw extruder squeeze out, pelletizing to get；When double screw extruder squeezes out, from
Peroxide master batch is added in the auxiliary spout of double screw extruder, controls main spout and assists the feeding quality speed of spout
Rate ratio is 100:1-100:10.
9. preparation method as claimed in claim 8, which is characterized in that each area's temperature of double screw extruder is set are as follows: Z1:
185-195 DEG C, Z2:205-215 DEG C, Z3:210-220 DEG C, Z4:215-225 DEG C, Z5:215-225 DEG C, Z6:210-220 DEG C, machine
Head: 205-215 DEG C, double-screw extruder screw revolving speed is 310rpm.
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| CN101619152A (en) * | 2009-07-30 | 2010-01-06 | 聊城大学 | High tenacity low smoke zero halogen flame retardant polypropylene and preparation method thereof |
| CN102146185A (en) * | 2010-02-04 | 2011-08-10 | 中国石油化工股份有限公司 | Controllable-rheological toughened transparent polypropylene and preparation method thereof |
| CN102532697A (en) * | 2010-12-30 | 2012-07-04 | 合肥杰事杰新材料股份有限公司 | High-toughness low-odor scratch-resistant polypropylene composition and preparation method thereof |
| CN105254999A (en) * | 2015-10-14 | 2016-01-20 | 中国石油化工股份有限公司 | Scratch-resistant high-impact polypropylene resin material and preparing method |
-
2017
- 2017-09-30 CN CN201710917787.1A patent/CN109593276A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619152A (en) * | 2009-07-30 | 2010-01-06 | 聊城大学 | High tenacity low smoke zero halogen flame retardant polypropylene and preparation method thereof |
| CN102146185A (en) * | 2010-02-04 | 2011-08-10 | 中国石油化工股份有限公司 | Controllable-rheological toughened transparent polypropylene and preparation method thereof |
| CN102532697A (en) * | 2010-12-30 | 2012-07-04 | 合肥杰事杰新材料股份有限公司 | High-toughness low-odor scratch-resistant polypropylene composition and preparation method thereof |
| CN105254999A (en) * | 2015-10-14 | 2016-01-20 | 中国石油化工股份有限公司 | Scratch-resistant high-impact polypropylene resin material and preparing method |
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Application publication date: 20190409 |