CN108864347A - The production method of PPR pipe PP Pipe Compound - Google Patents
The production method of PPR pipe PP Pipe Compound Download PDFInfo
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- CN108864347A CN108864347A CN201810650995.4A CN201810650995A CN108864347A CN 108864347 A CN108864347 A CN 108864347A CN 201810650995 A CN201810650995 A CN 201810650995A CN 108864347 A CN108864347 A CN 108864347A
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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
- 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
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/06—Propene
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
The invention discloses a kind of production methods of PPR pipe PP Pipe Compound, propylene and ethylene are placed in progress binary random copolymerization reaction in fluidized-bed reactor, and product is de-gassed and is granulated, wherein：The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.Invention catalyst system is by the synergistic effect of interior external electron donor, so that product has wider molecular weight distribution, product processing performance is substantially improved.
Description
Technical field
The present invention relates to polypropylene production technical fields, and in particular to the production method of PPR pipe PP Pipe Compound.
Background technique
Prohibited from China in 2000 used in New Dwelling galvanized pipe as water supply line after, it is PA tube, poly-
Ethylene has been in control tremendous development, at present total about 500,000 tons of country's PP-R pipe annual capacity, but with domestic 87.5 ten thousand tons/year
The market dosage of PP-R pipe is compared, and for domestic raw material there is also very big notch in terms of meeting the market demand, PP Pipe Compound is external
Interdependency is higher, and country is continuously increased the attention degree of watering plastic pipe, future market demand will it is steady in have increasing.
Currently, the production technology of mainstream PPR pipe material includes loop technology, three well oiled process and Ineos gas both at home and abroad
Phase technique, since PPR pipe material melt index is lower, therefore it is required that there is material wider molecular weight distribution to increase processability
Can, therefore PPR manufacturing enterprise passes through series connection 2 and the above reactor both at home and abroad, zonal control added hydrogen widens molecular weight
Distribution not yet retrieves the related patents that the production of PPR pipe PP Pipe Compound is realized using single reactor.Unipol technique polypropylene
It is still in the technological assimilation phase, the domestic technique is in PPR pipe production field still in industry blank, technology patent quotient institute
The catalyst of offer be Z-N series third generation SHAC205 catalyst and corresponding ADT electron donor, the catalyst system without
Form control function does not have the characteristic of wider molecular weight distribution, and is easier to hot localised points occur in reaction controlling.
The difficult point of single reactor polypropylene plant production PPR pipe PP Pipe Compound essentially consists in：（1）Hardly result in wider molecule
The product for measuring distribution, leads to product poor processability；（2）Impact strength is relatively low, it is difficult to meet the use of low temp area downstream；（3）
Ethylene distribution is uneven.
Summary of the invention
The purpose of the present invention is to provide a kind of production method of PPR pipe PP Pipe Compound, solve in the prior art using single
Reactor production Polypropylene for Pipes hardly results in the product of wider molecular weight distribution, so as to cause product poor processability
The problem of.
In order to solve the above technical problems, the present invention uses following technical scheme：
Propylene and ethylene are placed in fluidized-bed reactor and carry out binary randomly altogether by a kind of production method of PPR pipe PP Pipe Compound
Poly- reaction, and product is de-gassed and is granulated, wherein：
The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.
Preferably, the Cat-A catalyst is Z-N catalyst series.
Preferably, the Cat-A catalyst is with MgCl2For carrier, TiCl4For activated centre, internal electron donor is
Alkyl replaces bis- ethers of 1,3-, aryl to replace one or more of bis- ethers of 1,3-, succinic acid esters, malonate class formation
Compounding.
Preferably, the external electron donor D-A is to dicyclopentyl dimethoxyl silane, cyclohexyl methyl dimethoxy
One or more of base silane, diisopropyl dimethoxy silane, second, isobutyl dimethoxy silane compounding.
Preferably, the mass ratio of the ethylene and propylene is 3-5：95-97, can choose partial pressure of propylene is 1.5-
3.5Mpa, ethylene partial pressure position 0.04-0.09 Mpa；The catalyst solid flow is 0.30-0.70kg/h.
Preferably, wherein fluidized-bed reactor has one or phase using Unipol gas-phase polymerization polypropylene technology
Mutually concatenated two.
Preferably, the fluidized-bed reactor bed weight is 15-25t, height of bed 17-22m, superficial gas velocity 0.25-
0.45m/s。
Preferably, the H/C molar ratio is 0.0025-0.0065, Al/Ti molar ratio is 42-47, Al/Si mole
Than for 2.5-5.0.
Preferably, add additive co-extrusion in granulation step into the product after degassing and be granulated, the additive packet
It includes main anti-oxidant OA-1010 and OA-330, help antioxidant 0A-168, plumper calcium stearate, processing aid PPA and Beta
Nucleant agent N A-82.
Preferably, granulation step, main anti-oxidant OA-1010 2000-3500ppm is contained in material；Master is anti-oxidant
Agent OA-330 2000-3500ppm；Help antioxidant 0A-168 800-2000ppm；Calcium stearate 300-700ppm, processing help
Agent PPA 200-800ppm, nucleating agent 0-500ppm.
The application is carried out on the basis of unipol vapor phase method, process mainly include the purification of raw material, catalyst into
Material, polymerization, polymer degassing and tail gas recycle, granulation.Wherein, polymerization reaction system can be by one or two reaction
Device composition, by gaseous polymerization-grade propylene, ethylene, hydrogen and catalyst, triethyl aluminum, that electron donor is continuously added to fluidized bed is anti-
Device is answered, setup parameter is simultaneously reacted.
Compared with prior art, beneficial effects of the present invention are at least one of following：
Invention catalyst system is produced by the synergistic effect of interior external electron donor so that product has wider molecular weight distribution
Product processing performance is substantially improved.
The present invention is used only single fluidised bed reactor and successfully produces PPR pipe material, reduces equipment investment and is produced into
This, yield is up to 20t/h under this method.
The present invention passes through Optimization of Ethylene and nucleating agent additive amount, PPR pipe PP Pipe Compound impact with higher produced
Intensity and moderate bending modulus.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1：
The production method for present embodiments providing a kind of PPR pipe PP Pipe Compound, includes the following steps：
Catalyst solid flow is reduced to 0.52kg/h, adjusts partial pressure of propylene to 2Mpa, ethylene partial pressure to 0.05Mpa, reaction temperature
Degree is 72 DEG C, pressure 3.24Mpa, when reactor hydrogen partial pressure is 0.008Mpa, it is ensured that hydrogen-carbon ratio and Al/Ti control are flat
Surely.
When extrusion granulation powder melt index is 0.2g/10min, come into operation PPR pipe PP Pipe Compound of extrusion granulation unit is special
Determine additive, switch to finished product bin, wherein additive includes following components：Main anti-oxidant（1010）Add 3000ppm；It is main
Antioxidant（330）Add 3000ppm；Help antioxidant（168）Add 800ppm；Calcium stearate adds 500ppm, and processing helps
300ppm is added in agent (PPA), and nucleating agent (NA-82) adds 200ppm.
Reaction load is continuously improved and adjusts reactor hydrogen after granule product melt index and qualified isotacticity to 20t/h
Gas concentration makes the melt index of its final products maintain 0.2-0.3g/10min.
The catalyst is：Cat-A；
The external electron donor is：D-A；
The catalyst solid flow is 0.50kg/h；
The Al/Ti molar ratio is 45；
The ethylene additive amount is 4%；
The reactor beds weight is 18t, height of bed 19m, superficial gas velocity 0.35m/s；
The partial pressure of propylene is 2Mpa, ethylene partial pressure 0.05Mpa.
Embodiment 2：
The production method for present embodiments providing a kind of PPR pipe PP Pipe Compound, includes the following steps：
Catalyst solid flow is reduced to 0.52kg/h, adjusts partial pressure of propylene to 2Mpa, ethylene partial pressure to 0.06Mpa, reaction temperature
Degree is 72 DEG C, pressure 3.24Mpa, when reactor hydrogen partial pressure is 0.008Mpa, it is ensured that hydrogen-carbon ratio and Al/Ti control are flat
Surely.
When extrusion granulation powder melt index is 0.2g/10min, come into operation PPR pipe PP Pipe Compound of extrusion granulation unit is special
Determine additive, switch to finished product bin, wherein additive includes following components：Main anti-oxidant（1010）Add 3000ppm；It is main
Antioxidant（330）Add 3000ppm；Help antioxidant（168）Add 800ppm；Calcium stearate adds 500ppm, and processing helps
Agent PPA adds 300ppm, is not added with nucleating agent.
Reaction load is continuously improved and adjusts reactor hydrogen after granule product melt index and qualified isotacticity to 20t/h
Gas concentration makes the melt index of its final products maintain 0.2-0.3g/10min.
The catalyst is：Cat-A；
The external electron donor is：D-A；
The catalyst solid flow is 0.50kg/h；
The Al/Ti molar ratio is 45；
The ethylene additive amount is 4.5%；
The reactor beds weight is 18t, height of bed 19m, superficial gas velocity 0.35m/s；
The partial pressure of propylene is 2Mpa, 0.06 Mpa of ethylene partial pressure.
Embodiment 3：
A kind of production method of PPR pipe PP Pipe Compound, propylene and ethylene are placed in Unipol gas-phase polymerization polypropylene technology
Fluidized-bed reactor in carry out binary random copolymerization reaction, the fluidized-bed reactor bed weight be 15t, height of bed 17m, apparently
Gas velocity is 0.25m/s, and product is de-gassed and is granulated, wherein：
The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.
The Cat-A catalyst is Z-N catalyst series, and Z-N catalyst series are with MgCl2For carrier, TiCl4For work
Property center, internal electron donor is that alkyl replaces 1,3-, bis- ethers and aryl to replace 1,3-, bis- ethers；
The external electron donor D-A is to dicyclopentyl dimethoxyl silane and Cyclohexyl Methyl Dimethoxysilane；
In reaction process, partial pressure of propylene 1.5Mpa, 0.04 Mpa of ethylene partial pressure position；The catalyst solid flow is
0.30kg/h；The H/C molar ratio be 0.0025, Al/Ti molar ratio be 42, Al/Si molar ratio is 2.5.
In granulation step, additive co-extrusion is added into the product after degassing and is granulated, makes to contain main anti-oxidant in material
OA-1010 2000ppm；Main anti-oxidant OA-330 2000ppm；Help antioxidant 0A-168 800ppm；Calcium stearate
300ppm, processing aid PPA 200ppm.
Embodiment 4：
A kind of production method of PPR pipe PP Pipe Compound, propylene and ethylene are placed in Unipol gas-phase polymerization polypropylene technology
Fluidized-bed reactor in carry out binary random copolymerization reaction, the fluidized-bed reactor bed weight be 25t, height of bed 22m, apparently
Gas velocity is 0.45m/s, and product is de-gassed and is granulated, wherein：
The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.
The Cat-A catalyst is Z-N catalyst series, and Z-N catalyst series are with MgCl2For carrier, TiCl4For work
Property center, internal electron donor be alkyl replaced succinate esters；
The external electron donor D-A is diisopropyl dimethoxy silane；
In reaction process, partial pressure of propylene 3.5Mpa, 0.09 Mpa of ethylene partial pressure position；The catalyst solid flow is
0.70kg/h；The H/C molar ratio be 0.0065, Al/Ti molar ratio be 47, Al/Si molar ratio is 5.0.
In granulation step, additive co-extrusion is added into the product after degassing and is granulated, makes to contain main anti-oxidant in material
OA-1010 3500ppm；Main anti-oxidant OA-330 3500ppm；Help antioxidant 0A-1682000ppm；Calcium stearate
700ppm, processing aid PPA 800ppm, nucleating agent 500ppm.
Embodiment 5：
A kind of production method of PPR pipe PP Pipe Compound, propylene and ethylene are placed in Unipol gas-phase polymerization polypropylene technology
Fluidized-bed reactor in carry out binary random copolymerization reaction, the fluidized-bed reactor bed weight be 20t, height of bed 20m, apparently
Gas velocity is 0.3m/s, and product is de-gassed and is granulated, wherein：
The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.
The Cat-A catalyst is Z-N catalyst series, and Z-N catalyst series are with MgCl2For carrier, TiCl4For work
Property center, internal electron donor be malonate class formation；
The external electron donor D-A is dicyclopentyl dimethoxyl silane；
In reaction process, partial pressure of propylene 2.5Mpa, 0.07 Mpa of ethylene partial pressure position；The catalyst solid flow is
0.50kg/h；The H/C molar ratio be 0.0045, Al/Ti molar ratio be 45, Al/Si molar ratio is 3.5.
In granulation step, additive co-extrusion is added into the product after degassing and is granulated, makes to contain main anti-oxidant in material
OA-1010 3000ppm；Main anti-oxidant OA-330 3000ppm；Help antioxidant 0A-168 1500ppm；Calcium stearate
500ppm, processing aid PPA 500ppm, nucleating agent 250ppm.
It is tested by five kinds of products that embodiment 1-5 is obtained, product Key Quality Indicator see the table below：
| Serial number | Project | Index request | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| 1 | Melt mass flow rate | 0.2-0.4g/10min | 0.25 | 0.25 | 0.25 | 0.25 | 0.25 |
| 2 | Bending modulus | ≥650Mpa | 679 | 690 | 690 | 696 | 713 |
| 3 | Simply supported beam notch impact strength（23℃） | ≥40KJ/m2 | 75 | 70 | 72 | 74 | 79 |
| 4 | Stretching yield stress | ≥23Mpa | 27 | 27 | 27 | 28 | 29 |
| 5 | Melting temperature | ≤146℃ | 135 | 138 | 136 | 140 | 141 |
| 6 | Molecular weight distribution | ≥4.5 | 6.8 | 6.9 | 6.8 | 7.0 | 7.3 |
| 7 | Yellow colour index | ≤0 | -3.2 | -3.0 | -3.0 | -3.1 | -3.3 |
| 8 | Load deformation temperature | ≥60℃ | 67 | 69 | 70 | 69 | 73 |
As can be seen from Table 1, the produced product of inventive formulation has reached higher in terms of molecular weight distribution, impact strength
Level, and all indexs are superior to professional standard, and product quality is adjustable.
Although reference be made herein to invention has been described for multiple explanatory embodiments of the invention, however, it is to be understood that
Those skilled in the art can be designed that a lot of other modification and implementations, these modifications and implementations will fall in this Shen
It please be within disclosed scope and spirit.It more specifically, within the scope of the present disclosure and claims, can be to master
The building block and/or layout for inscribing composite configuration carry out a variety of variations and modifications.In addition to what is carried out to building block and/or layout
Outside modification and improvement, to those skilled in the art, other purposes also be will be apparent.
Claims (10)
1. a kind of production method of PPR pipe PP Pipe Compound, it is characterised in that：By propylene and ethylene be placed in fluidized-bed reactor into
Row binary random copolymerization reaction, and product is de-gassed and is granulated, wherein：
The copolyreaction of propylene and ethylene carries out under Cat-A catalyst and external electron donor D-A collective effect.
2. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the Cat-A catalyst is
Z-N catalyst series.
3. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the Cat-A catalyst is
With MgCl2For carrier, TiCl4For activated centre, internal electron donor is that alkyl replaces 1,3-, bis- ethers, aryl to replace 1,3- diether
One or more of class, succinic acid esters, malonate class formation compounding.
4. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the external electron donor D-A
For to dicyclopentyl dimethoxyl silane, Cyclohexyl Methyl Dimethoxysilane, diisopropyl dimethoxy silane, diisobutyl
One or more of dimethoxysilane compounding.
5. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the ethylene and propylene
Mass ratio is 3-5：95-97；The catalyst solid flow is 0.30-0.70kg/h.
6. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that use Unipol vapor phase method
Polymarization method for prodcing polyacrylates technology, wherein fluidized-bed reactor have one or be serially connected two.
7. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the fluidized-bed reactor
Bed weight is 15-25t, height of bed 17-22m, superficial gas velocity 0.25-0.45m/s.
8. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that the H/C molar ratio is
0.0025-0.0065, Al/Ti molar ratio are that 42-47, Al/Si molar ratio are 2.5-5.0.
9. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that in granulation step, to degassing
In product afterwards add additive co-extrusion be granulated, the additive include main anti-oxidant OA-1010 and OA-330, help it is anti-oxidant
Agent 0A-168, plumper calcium stearate, processing aid PPA and Beta nucleant agent N A-82.
10. the production method of PPR pipe PP Pipe Compound according to claim 1, which is characterized in that granulation step, in material
Contain main anti-oxidant OA-1010 2000-3500ppm；Main anti-oxidant OA-330 2000-3500ppm；Help antioxidant
0A-168 800-2000ppm；Calcium stearate 300-700ppm, processing aid PPA 200-800ppm, nucleating agent 0-
500ppm。
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| CN201810650995.4A CN108864347B (en) | 2018-06-22 | 2018-06-22 | Production method of special material for PPR (polypropylene random copolymer) pipe |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437358A (en) * | 2019-07-03 | 2019-11-12 | 联泓新材料科技股份有限公司 | A kind of high polyacrylic preparation method of thin-walled injection moulding thoroughly of high-ductility |
| CN110437359A (en) * | 2019-07-03 | 2019-11-12 | 联泓新材料科技股份有限公司 | A kind of polyacrylic preparation method of milky tea cup |
| CN111303319A (en) * | 2020-03-13 | 2020-06-19 | 云南云天化石化有限公司 | Production method of medium and high melt index warp-resistant polypropylene special material |
| CN111303327A (en) * | 2020-03-13 | 2020-06-19 | 云南云天化石化有限公司 | Special high-transparency food-grade polypropylene material and production method 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 |
| CN115304867A (en) * | 2021-05-06 | 2022-11-08 | 中国石油天然气股份有限公司 | Special resin for toughened PPR (polypropylene random copolymer) pipe and preparation method thereof |
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| CN106749820A (en) * | 2016-11-25 | 2017-05-31 | 联泓新材料有限公司 | A kind of production method of atactic copolymerized polypropene |
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- 2018-06-22 CN CN201810650995.4A patent/CN108864347B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106749820A (en) * | 2016-11-25 | 2017-05-31 | 联泓新材料有限公司 | A kind of production method of atactic copolymerized polypropene |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437358A (en) * | 2019-07-03 | 2019-11-12 | 联泓新材料科技股份有限公司 | A kind of high polyacrylic preparation method of thin-walled injection moulding thoroughly of high-ductility |
| CN110437359A (en) * | 2019-07-03 | 2019-11-12 | 联泓新材料科技股份有限公司 | A kind of polyacrylic preparation method of milky tea cup |
| CN110437358B (en) * | 2019-07-03 | 2022-04-22 | 联泓新材料科技股份有限公司 | Preparation method of high-toughness high-transparency thin-wall injection molding polypropylene |
| CN111303319A (en) * | 2020-03-13 | 2020-06-19 | 云南云天化石化有限公司 | Production method of medium and high melt index warp-resistant polypropylene special material |
| CN111303327A (en) * | 2020-03-13 | 2020-06-19 | 云南云天化石化有限公司 | Special high-transparency food-grade polypropylene material and production method 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 |
| CN115304867A (en) * | 2021-05-06 | 2022-11-08 | 中国石油天然气股份有限公司 | Special resin for toughened PPR (polypropylene random copolymer) pipe and preparation method thereof |
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