CN102850663B - A kind of low temperature resistant polypropylene random copolymer material, preparation method and applications - Google Patents
A kind of low temperature resistant polypropylene random copolymer material, preparation method and applications Download PDFInfo
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- CN102850663B CN102850663B CN201110179003.2A CN201110179003A CN102850663B CN 102850663 B CN102850663 B CN 102850663B CN 201110179003 A CN201110179003 A CN 201110179003A CN 102850663 B CN102850663 B CN 102850663B
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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
- B29C48/04—Particle-shaped
Abstract
The invention belongs to technical field of polymer composite materials, disclose a kind of low temperature resistant polypropylene random copolymer material, preparation method and applications.Polypropylene random copolymer material disclosed by the invention includes following components and weight portion: 70 100 parts of atactic copolymerized polypropenes, 0.01 1 parts of beta nucleaters, 2 15 parts of POEs, 1 15 parts of inorganic fillers and 0.1 0.6 parts of antioxidant.The preparation method of this polypropylene random copolymer material comprises the following steps: by 70 100 parts of atactic copolymerized polypropenes, 0.01 1 parts of beta nucleaters, 2 15 parts of POEs, 1 15 parts of inorganic fillers and 0.1 0.6 parts of antioxidant, put into and in super mixer, be dry mixed 35 minutes, the raw material extruder mixing is melt extruded, granulation.A kind of method that polypropylene random copolymer material is prepared as PPR pipe, the method comprises the following steps: the polypropylene random copolymer material that will prepare, and is processed into PPR pipe with PPR pipe production line.Under the material at low temperature of the present invention, impact strength is very high, and resistance to low temperature is good.
Description
Technical field
The invention belongs to technical field of polymer composite materials, relate to a kind of low temperature resistant polypropylene random copolymer material, system
Preparation Method and application thereof.
Background technology
Atactic copolymerized polypropene (PPR), to being again three type PA tubes, polypropylene random copolymer pipe, is to be gathered by random copolymerization
Propylene special material for tube is extruded to be processed.PPR pipe is good, corrosion-resistant except having general plastic pipe light weight, intensity
Outside with advantages such as length in service life, also having the advantage that inner wall smooth, flow resistance is little and non-scaling；Operation letter is installed
Folk prescription just, has solderability, can in seconds weld together；PPR pipe is at the waste product producing and produce in construction work
Recoverable, can reduce production cost, free from environmental pollution；Heat resistance is good, and maximum operating temperature can reach 95 DEG C,
Under 1.0MPa pressure, Long-Time Service temperature is up to 70 DEG C.
Polypropylene random copolymer is typically to be passed through propylene and other a small amount of monomers, predominantly second in a reactor
Alkene, also carries out what random copolymerization obtained with 1-butylene and 1-hexene sometimes.In general random copolymer, the quality of comonomer is divided
Number is 1%-7%.Atactic copolymerized polypropene compared with HOPP, the tensile strength of random copolymer, modulus, hardness and heat
Deformation temperatures etc. all decrease, but impact strength and the transparency are improved.The phase of speciality propylene random copolymer for tubing
High to molecular mass, melt index ＜ 0.5g/10min, thus have good mechanical performance.Again owing to ethene is randomly-embedded propylene
In long-chain, increase intermolecular winding performance, thus there is splendid environmental stress crack resistance and creep resistance.
PPR pipe embrittlement at low temperatures is one of its shortcoming, and its brittle temperature is about-10 DEG C, thus temperature in winter
It when very low, is easily damaged in transport and installation process.Therefore, the low temperature punching of PPR pipe how is improved further
Hitting performance has become a problem with very high practical value.
For this problem, Fu Qiang, Luo Feng, Wang Ke etc. are to mention in CN101891923A patent first in patent publication No.
Atactic copolymerized polypropene and beta nucleater melt blending make beta nucleater masterbatch, and then beta nucleater masterbatch adds to random being total to
In poly-polypropylene, melt blending makes the atactic copolymerized polypropene modified pellet under low temperature with excellent toughness.But, beta nucleater
At the limited extent improving atactic copolymerized polypropene low-temperature flexibility.
Content of the invention
In order to overcome the defect of PPR pipe low temperature embrittlement, it is an object of the invention to provide a kind of low temperature resistant random copolymerization and gather
Propylene material, this material at low temperature impact strength is very high, and resistance to low temperature is good.
It is a further object to provide the preparation method of a kind of above-mentioned low temperature resistant polypropylene random copolymer material.
Third object of the present invention is to provide one and above-mentioned low temperature resistant polypropylene random copolymer material is prepared as PPR pipe
The method of material.
Technical scheme is as follows:
The invention provides a kind of low temperature resistant polypropylene random copolymer material, this material includes following components and weight portion:
Atactic copolymerized polypropene 70-100 part,
Beta nucleater 0.01-1 part,
Ethylene-octene copolymer 2-15 part,
Inorganic filler 1-15 part,
Antioxidant 0.1-0.6 part.
Described atactic copolymerized polypropene (PPR) is the ethylene-propylene random copolymer that ethylene contents is 3%-5%, weight
Average molecular weight is more than 500,000, and melt index is less than 0.5g/10min.Described beta nucleater is selected from aromatic amides class beta nucleater
Or the brilliant nucleator of rare earth compounding β.
Described ethylene-octene copolymer (POE) is linear ethylene-octene copolymer, and density is 0.88-0.90g/cm3,
Melt index is 1-50g/10min.
One or more in talcum powder, calcium carbonate or barium sulfate of described inorganic filler.
Described antioxidant includes primary antioxidant and auxiliary anti-oxidant, and primary antioxidant is selected from hindered phenol or sulphur ester antioxidant
One or more, be further selected from four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester
(antioxidant 1010)；Auxiliary anti-oxidant is selected from phosphite antioxidant, is further selected from three [2.4-di-tert-butyl-phenyl] phosphorous acid
Ester (irgasfos 168).
Present invention also offers the preparation method of a kind of above-mentioned low temperature resistant polypropylene random copolymer material, the method include with
Lower step:
By 70-100 part atactic copolymerized polypropene, 0.01-1 part beta nucleater, 2-15 part ethylene-octene copolymer, 1-15 part
Inorganic filler and 0.1-0.6 part antioxidant, put into and 3-5 minute be dry mixed in super mixer, the raw material extruder that will mix
Melt extrude, granulation.
Described extruder is double screw extruder, feed zone temperature 160-180 DEG C, and compression section temperature 180-200 DEG C is moulded
Change section temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Present invention also offers a kind of method that above-mentioned low temperature resistant polypropylene random copolymer material is prepared as PPR pipe,
The method comprises the following steps: the polypropylene random copolymer material that will prepare, and is processed into PPR pipe with PPR pipe production line
Material.
The extrusion temperature of described PPR pipe production line is: a district: 150-180 DEG C, 2nd district: 190-200 DEG C, 3rd district:
200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, cooling water temperature 15-20 DEG C, and cooling and shaping vacuum is
0.4MPa。
The present invention compared with prior art, has the advantage that and beneficial effect:
1st, the present invention is by adding beta nucleater and ethylene-octene copolymer simultaneously so that polypropylene random copolymer material
Under low temperature, impact strength is very high, and resistance to low temperature is good.
2nd, the rigidity that the present invention is brought because of the raising of resistance to low temperature by adding a small amount of inorganic filler to solve declines
Problem.
3rd, the one low temperature resistant PPR pipe preparation technology that the present invention proposes is simple, and production cost is low.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
In embodiment and comparative example are filled a prescription, PPR is the atactic copolymerized polypropene that Daqing Refinery company produces, trade names
For PA14D, its melt index is 0.33g/10min (230 DEG C, 2.16kg), atactic copolymerized polypropene be ethylene contents be 3%-
The ethylene-propylene random copolymer of 5%, weight average molecular weight is more than 500,000.Aromatic amides class beta nucleater used is Shanxi
The brilliant nucleator of the graduate TMB-4 of work, rare earth compounding β used is the WBG-A of Guangzhou Wei Linna functional material Co., Ltd.
POE used is E.I.Du Pont Company's product 8150, and ethylene-octene copolymer (POE) is linear ethylene-octene copolymer, and density is
0.88-0.90g/cm3, melt index is 1-50g/10min.Talcous particle size range used is 10 microns.Used
Calcium carbonate is nano-calcium carbonate, and its particle size range is 40 nanometers.Primary antioxidant used is Ciba's product antioxidant
1010, chemical name is four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester.Auxiliary anti-oxidant
For Ciba's product irgasfos 168, chemical name is three [2.4-di-tert-butyl-phenyl] phosphite ester.
Embodiment 1
By 70 parts of atactic copolymerized polypropene PA14D, 0.01 part of nucleator TMB-4,15 parts of POE the 8150th, 10 parts of talcum powder, 5
Part nano-calcium carbonate, 0.1 part of antioxidant 1010, put into and 3-5 minute be dry mixed in super mixer, the raw material that will mix pair spiral shells
Bar extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section temperature 180-200 DEG C,
Fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Embodiment 2
By 80 parts of atactic copolymerized polypropene PA14D, 0.1 part of nucleator TMB-4,8 parts of POE the 8150th, 8 parts of talcum powder, 0.1
Part antioxidant 1010,0.2 part of irgasfos 168, put into and 3-5 minute be dry mixed in super mixer, the raw material that will mix pair spiral shells
Bar extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section temperature 180-200 DEG C,
Fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Embodiment 3
By 85 parts of atactic copolymerized polypropene PA14D, 0.05 part of nucleator TMB-4,5 parts of POE the 8150th, 5 parts of talcum powder, 5 parts
Nano-calcium carbonate, 0.15 part of antioxidant 1010,0.25 part of irgasfos 168 are put into and 3-5 minute are dry mixed in super mixer, will mixing
Good raw material double screw extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section
Temperature 180-200 DEG C, fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Embodiment 4
By 91 parts of atactic copolymerized polypropene PA14D, 0.5 part of nucleator WBG-A, 2 parts of POE the 8150th, 5 parts of talcum powder, 0.1
Part antioxidant 1010,0.2 part of irgasfos 168, put into and 3-5 minute be dry mixed in super mixer, the raw material that will mix pair spiral shells
Bar extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section temperature 180-200 DEG C,
Fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Embodiment 5
By 94 parts of atactic copolymerized polypropene PA14D, 1 part of nucleator WBG-A, 5 parts of POE the 8150th, 1 part of talcum powder, 0.1 part
Antioxidant 1010,0.2 part of irgasfos 168, put into and 3-5 minute be dry mixed in super mixer, the raw material twin-screw that will mix
Extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section temperature 180-200 DEG C, mould
Change section temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Embodiment 6
By 100 parts of atactic copolymerized polypropene PA14D, 0.2 part of nucleator TMB-4,3 parts of POE the 8150th, 1 part of nano-calcium carbonates
Calcium, 0.2 part of antioxidant 1010,0.2 part of irgasfos 168 are put into and 3-5 minute are dry mixed in super mixer, use the raw material mixing
Double screw extruder melt extrudes, granulation.Feed zone temperature 160-180 DEG C of double screw extruder, compression section temperature 180-200
DEG C, fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Comparative example
100 parts of atactic copolymerized polypropene PA14D, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168 are put into mixed at high speed
3-5 minute is dry mixed in device, the raw material double screw extruder mixing is melt extruded, granulation.The charging of double screw extruder
Duan Wendu 160-180 DEG C, compression section temperature 180-200 DEG C, fluxing zone temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C,
Die temperature 190-210 DEG C.
Again the pellet PP-R pipe production line having granulated is processed into PPR pipe.Extrusion temperature is: a district: 150-180
DEG C, 2nd district: 190-200 DEG C, 3rd district: 200-210 DEG C, 4th district: 200-220 DEG C, mold temperature is 190-210 DEG C, coolant water temperature
Spending 15-20 DEG C, cooling and shaping vacuum is 0.4MPa.The performance test results is shown in Table 1.
Performance evaluation mode and implementation standard:
By the good particle of above-mentioned granulation, the convection oven of 90-100 DEG C is dried 2-3 hour, then at injection moulding machine
Upper injection mo(u)lding sample preparation.
Tensile property test is carried out by ISO 527-2；Bending property is carried out by ISO 178；Cantilever beam impact strength presses ISO
180 are carried out；Tubing hydrostatic test is carried out by GBT 18742.
Table 1
From embodiment 1-6 and comparative example it can be seen that by add beta nucleater, POE, PPR pipe PP Pipe Compound PA14D-
The low temperature impact strength of 20 DEG C is improved, and than comparative example, former PA14D divides the low-temperature flexibility of-20 DEG C of embodiment 1-6 respectively
Do not improve the 93%th, the 77%th, the 47%th, the 40%th, the 43%th, 23%.And the bending modulus of embodiment 1-6 is compared with comparative example, base
Not reducing in basis, some improve on the contrary, show that the rigidity of material does not decline.In hydrostatic test, all of enforcement
Example has all passed through detection, illustrates to the addition of the pressure performance that beta nucleater, POE, filler do not affect tubing.In a word, by improving
Low-temperature flexibility, tubing just can remain to keep preferable toughness at low temperatures, it is simple to transport and installation under extremely low temperature condition, solves
Determine the difficult problem of PPR low temperature embrittlement.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply this
Bright.These embodiments obviously easily can be made various modification by person skilled in the art, and described herein
General Principle is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to enforcement here
Example, those skilled in the art are according to the announcement of the present invention, and the improvement made without departing from scope and modification all should be
Within protection scope of the present invention.
Claims (6)
1. a polypropylene random copolymer material, it is characterised in that: this material includes following components and weight portion:
Described atactic copolymerized polypropene is the ethylene-propylene random copolymer that ethylene contents is 3%-5%, and weight average molecular weight exists
More than 500000, melt index is less than 0.5g/10min；
Described beta nucleater is selected from aromatic amides class beta nucleater TMB-4；
Described ethylene-octene copolymer is linear ethylene-octene copolymer, and density is 0.88-0.90g/cm3, melt index is
1-50g/10min；
One or more in talcum powder, calcium carbonate or barium sulfate of described inorganic filler；
The preparation method of described polypropylene random copolymer material comprises the steps of:
By inorganic to 70-100 part atactic copolymerized polypropene, 0.01-1 part beta nucleater, 2-15 part ethylene-octene copolymer, 1-15 part
Filler and 0.1-0.6 part antioxidant, put into and 3-5 minute be dry mixed in super mixer, melts the raw material extruder mixing
Extrusion, granulation；
Described extruder is double screw extruder, feed zone temperature 160-180 DEG C, compression section temperature 180-200 DEG C, fluxing zone
Temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
2. polypropylene random copolymer material according to claim 1, it is characterised in that: described antioxidant includes main antioxygen
Agent and auxiliary anti-oxidant, primary antioxidant is selected from one or more in hindered phenol or sulphur ester antioxidant, and auxiliary anti-oxidant is selected from phosphorous
Acid esters antioxidant.
3. polypropylene random copolymer material according to claim 2, it is characterised in that: described primary antioxidant is selected from four
[methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester.
4. polypropylene random copolymer material according to claim 2, it is characterised in that: described auxiliary anti-antioxidant is selected from three
[2,4-di-tert-butyl-phenyl] phosphite ester.
5. the preparation method of the arbitrary described polypropylene random copolymer material of Claims 1-4, it is characterised in that: the method bag
Include following steps:
By inorganic to 70-100 part atactic copolymerized polypropene, 0.01-1 part beta nucleater, 2-15 part ethylene-octene copolymer, 1-15 part
Filler and 0.1-0.6 part antioxidant, put into and 3-5 minute be dry mixed in super mixer, melts the raw material extruder mixing
Extrusion, granulation；
Described extruder is double screw extruder, feed zone temperature 160-180 DEG C, compression section temperature 180-200 DEG C, fluxing zone
Temperature 180-210 DEG C, homogenizing zone temperature 200-220 DEG C, die temperature 190-210 DEG C.
6. arbitrary for Claims 1-4 described polypropylene random copolymer material is prepared as the method for PPR pipe, and its feature exists
In: the method comprises the following steps: the polypropylene random copolymer material that will prepare, and is processed into PPR with PPR pipe production line
Tubing.
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| CN105623073A (en) * | 2014-10-27 | 2016-06-01 | 中国石油天然气股份有限公司 | Method for improving properties of polypropylene material or product thereof |
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| CN113402753A (en) * | 2020-07-31 | 2021-09-17 | 江苏品升管业股份有限公司 | Processing method of cold-resistant pipeline |
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| CN112976626A (en) * | 2021-01-28 | 2021-06-18 | 中裕软管科技股份有限公司 | Manufacturing process of light, bendable and high and low temperature resistant spiral water suction pipe |
| CN114989604A (en) * | 2021-03-01 | 2022-09-02 | 中国石油化工股份有限公司 | Pipe composition, preparation method and application thereof |
| CN115304699A (en) * | 2021-05-06 | 2022-11-08 | 中国石油天然气股份有限公司 | Special resin for PPR (polypropylene random copolymer) pipe and preparation method thereof |
| CN114479284B (en) * | 2021-12-13 | 2022-12-13 | 华南理工大学 | PP-RCT special material and pipe with high beta crystal content and preparation method thereof |
| CN114440013B (en) * | 2021-12-28 | 2024-04-05 | 日丰企业集团有限公司 | Low-temperature-resistant PP-R composite pipe and preparation method and application thereof |
| CN114806024A (en) * | 2022-05-05 | 2022-07-29 | 横店集团得邦工程塑料有限公司 | High-impact-resistance low-temperature-resistance polypropylene material and preparation method thereof |
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| CN101245228A (en) * | 2008-02-29 | 2008-08-20 | 广州市合诚化学有限公司 | Hot melt adhesive special for random copolymerization polypropylene multiunit tube and manufacture method thereof |
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| CN101891923A (en) * | 2010-07-30 | 2010-11-24 | 四川大学 | Method for preparing low-temperature flexible random copolymerization polypropylene product |
| CN102002189A (en) * | 2010-12-10 | 2011-04-06 | 上海金发科技发展有限公司 | High and low temperature toughness modified polypropylene material and preparation method thereof |
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