CN111333754A - Method for preparing polypropylene resin with large melt index - Google Patents

Method for preparing polypropylene resin with large melt index Download PDF

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Publication number
CN111333754A
CN111333754A CN202010310091.4A CN202010310091A CN111333754A CN 111333754 A CN111333754 A CN 111333754A CN 202010310091 A CN202010310091 A CN 202010310091A CN 111333754 A CN111333754 A CN 111333754A
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China
Prior art keywords
block
degree
degree shear
shear block
section
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CN202010310091.4A
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Chinese (zh)
Inventor
穆肖斌
李骥安
王涛
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SHANGHAI FUNCTIONAL POLYMER MATERIAL RESEARCH INSTITUTE
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SHANGHAI FUNCTIONAL POLYMER MATERIAL RESEARCH INSTITUTE
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Priority to CN202010310091.4A priority Critical patent/CN111333754A/en
Publication of CN111333754A publication Critical patent/CN111333754A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00Chemical modification by after-treatment
    • C08F8/50Partial depolymerisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/02Making granules by dividing preformed material
    • B29B9/06Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion

Abstract

The invention relates to the technical field of polypropylene resin preparation, in particular to a method for preparing polypropylene resin with large melt index. Compared with the prior art, the invention adopts the steps of accurately controlling the feeding amount of the polypropylene and the injection amount of the oxygen, and the sectional heating and shearing action, so that the polypropylene passing through the extruder in unit time is completely subjected to the same action, and the discharged melt fingers are very uniform. No additive is added in the preparation process, only physical action is generated in the extrusion process, the production process is environment-friendly, and the generated polypropylene resin is clean and safe and can be applied to the field of sanitary materials or other materials with ultra-clean requirements.

Description

Method for preparing polypropylene resin with large melt index
Technical Field
The invention relates to the technical field of polypropylene resin preparation, in particular to a method for preparing polypropylene resin with large melt index.
Background
There are several methods for preparing polypropylene resin with large melt index, one is to control the molecular weight and molecular weight distribution of polypropylene by controlling the polymerization reaction process, for example, to increase the melt index by decreasing the molecular weight of the polymer by increasing the concentration of polymerization inhibitor, such as hydrogen. The method is limited by factors such as a catalytic system, reaction conditions and the like, the stability of the melt index is difficult to control, the implementation is difficult, and petrochemical enterprises have no mass polymerization. Another method is to control the degradation of polypropylene obtained by conventional polymerization, reduce the molecular weight and improve the melt index. In the past, the molecular weight of polypropylene is reduced by a common high-temperature degradation method, but the high-temperature degradation method has many defects, such as limited molecular weight reduction range, unstable process and the like. In addition, ultrasonic degradation methods are available, but these methods often require the presence of solvents, which increases the difficulty and cost of the process.
In recent years, a method of chemically degrading polypropylene has been used, in which polypropylene is reacted with a chemical initiator such as an organic peroxide in a screw extruder to break molecular chains of polypropylene and reduce the molecular weight thereof to increase the melt index. However, this process often contains residues of initiator and its decomposition products, which affect the field of use.
Therefore, it is necessary to design a method for preparing a polypropylene resin with large melt index, which can degrade polypropylene without adding an initiator, reduce molecular weight and improve melt index.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing polypropylene resin with large melt index, which can realize the degradation of polypropylene, reduce the molecular weight and improve the melt index without adding any auxiliary agent.
In order to achieve the above object, the present invention is a method for preparing a macromelt polypropylene resin, characterized in that: the method comprises the following steps: step 1, feeding polypropylene particles into a feeding section of a co-rotating double-screw extruder through a feeding port, wherein the temperature of the feeding section is 100-120 ℃, and under the action of a forward conveying block and a feeding section shearing block of the feeding section, the polypropylene particles are heated and are compressed and fed to a plasticizing section; step 2, injecting industrial oxygen with the pressure of 0.1-1.0 Mpa into a gas injection port of the plasticizing section, fully contacting and mixing the molten polypropylene and the industrial oxygen at the temperature of 180-280 ℃, degrading the molten polypropylene under the action of a shearing block of the plasticizing section and a reverse conveying block of the plasticizing section, and conveying the degraded polypropylene to a gas exhaust section; step 3, discharging residual oxygen from an exhaust port under the action of an exhaust section shearing block, an exhaust section reverse conveying block and an exhaust section forward conveying block at the temperature of 160-180 ℃, and conveying degraded polypropylene to a metering section; and 4, extruding the degraded polypropylene into strips from a machine head and a mouth die at the temperature of 140-160 ℃ under the action of a forward conveying block of the metering section, cooling by a water tank, pelletizing and drying to form large melt index polypropylene particles.
The diameter of a screw of the co-rotating double-screw extruder is 20 mm-120 mm, and the length-diameter ratio is 28-52.
The melt index of the polypropylene particles is 2-100 g/10min, and the melt index of the large melt index polypropylene particles after extrusion granulation is 15-2500 g/10 min.
The feeding section forward conveying block and the feeding section shearing block comprise a 48mm forward conveying block I, a 64mm forward conveying block I, 3 48mm forward conveying blocks II, a 64mm forward conveying block II, 2 48mm forward conveying blocks III, a 30-degree shearing block I and a 45-degree shearing block I which are arranged from front to back; the plasticizing section shear block and the plasticizing section reverse conveying block comprise a first 60-degree shear block, a first 90-degree shear block, a first 32-mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a second 32-mm reverse conveying block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a third 32-mm reverse conveying block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a fourth 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block, a fifth 32-mm reverse conveying block and a sixth 30-degree shear block; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block six, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
The feeding section forward conveying block and the feeding section shearing block comprise a 48mm forward conveying block I, a 64mm forward conveying block I, 3 48mm forward conveying blocks II, a 64mm forward conveying block II, 3 48mm forward conveying blocks III and a 30-degree shearing block I which are arranged from front to back; the plasticizing section shear block and the plasticizing section reverse conveying block comprise a first 45-degree shear block, a first 60-degree shear block, a first 90-degree shear block, a first 32mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a second 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block and a sixth 30-degree shear block which are arranged from front to back; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block three, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
Compared with the prior art, the polypropylene is degraded to different degrees by the combination and the combined action of the screw structure arrangement of the co-rotating double-screw extruder, the heating temperature setting and the oxygen introduction in the polypropylene extrusion process, the molecular weight is reduced, the melt index is improved, and the polypropylene resins with different grades are generated, so that the polypropylene resin can be applied to different occasions. Because the feeding amount of the polypropylene, the injection amount of the oxygen and the sectional heating and shearing action are accurately controlled, the polypropylene passing through the extruder in unit time is completely under the same action, and the melt index of discharging is very uniform. No additive is added in the preparation process, only physical action is generated in the extrusion process, the production process is environment-friendly, and the generated polypropylene resin is clean and safe and can be applied to the field of sanitary materials or other materials with ultra-clean requirements.
Drawings
FIG. 1 is a first block diagram of a screw of a co-rotating twin-screw extruder according to the present invention.
FIG. 2 is a second view showing the structure of a screw of the co-rotating twin-screw extruder of the present invention.
Detailed Description
The invention will now be further described with reference to the accompanying drawings.
The invention relates to a method for preparing polypropylene resin with large melt index, which comprises the following steps: step 1, feeding polypropylene particles into a feeding section 4 of a co-rotating twin-screw extruder through a feeding port 1, wherein the temperature of the feeding section is 100-120 ℃, and under the action of a forward conveying block and a feeding section shearing block of the feeding section, the polypropylene particles are heated and are compressed and conveyed to a plasticizing section 5; step 2, injecting industrial oxygen with the pressure of 0.1-1.0 Mpa into a gas injection port 2 of the plasticizing section, fully contacting and mixing the molten polypropylene and the industrial oxygen at the temperature of 180-280 ℃, degrading the molten polypropylene under the action of a shearing block of the plasticizing section and a reverse conveying block of the plasticizing section, and conveying the degraded polypropylene to an exhaust section 6; step 3, discharging residual oxygen from the exhaust port 3 under the action of the exhaust section shearing block, the exhaust section reverse conveying block and the exhaust section forward conveying block at the temperature of 160-180 ℃, and conveying degraded polypropylene to a metering section 7; and 4, extruding the degraded polypropylene into strips from a machine head and a mouth die at the temperature of 140-160 ℃ under the action of a forward conveying block of the metering section, cooling by a water tank, pelletizing and drying to form large melt index polypropylene particles.
The diameter of a screw of the co-rotating double-screw extruder is 20 mm-120 mm, and the length-diameter ratio is 28-52.
The melt index of the polypropylene particles is 2-100 g/10min, and the melt index of the large melt index polypropylene particles after extrusion granulation is 15-2500 g/10 min.
Example 1:
referring to FIG. 1, a co-rotating twin screw extruder having a diameter of 48mm and a length to diameter ratio of 48 was used in this example, in the following arrangement of high shear flights: the feeding section forward conveying block and the feeding section shearing block comprise a 48mm forward conveying block I, a 64mm forward conveying block I, 3 48mm forward conveying blocks II, a 64mm forward conveying block II, 2 48mm forward conveying blocks III, a 30-degree shearing block I and a 45-degree shearing block I which are arranged from front to back; the plasticizing section shear block and the plasticizing section reverse conveying block comprise a first 60-degree shear block, a first 90-degree shear block, a first 32mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a second 32-mm reverse conveying block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a third 32-mm reverse conveying block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a fourth 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block, a fifth 32-mm reverse conveying block and a sixth 30-degree shear block; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block six, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
In this example, the melt index of polypropylene is 100g/10min, the temperature of the three zones from the front to the back of the feeding section 4 is 100.0 ℃, 100.0 ℃ and 110.0 ℃, the temperature of the six zones from the front to the back of the plasticizing section 5 is 180.0 ℃, 250.0 ℃, 200.0 ℃, the injection pressure of industrial oxygen is 0.15MPa, the temperature of the two zones from the front to the back of the exhaust section 6 is 180.0 ℃, 160.0 ℃, the temperature of the metering section 7 is 140 ℃, and the polypropylene formed by extrusion is prepared, wherein the melt index is: 2500g/10 min.
Example 2:
referring to FIG. 1, a co-rotating twin screw extruder, 48mm diameter, 48 aspect ratio, medium shear flighting arrangement, is used in this example, as follows: the feeding section forward conveying block and the feeding section cutting block comprise a first 48mm forward conveying block, a first 64mm forward conveying block, 3 second 48mm forward conveying blocks, a second 64mm forward conveying block, a third 3 48mm forward conveying block and a first 30-degree cutting block which are arranged from front to back; the plasticized section shear block and the plasticized section reverse conveying block comprise a first 45-degree shear block, a first 60-degree shear block, a first 90-degree shear block, a first 32mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a second 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block and a sixth 30-degree shear block which are arranged from front to back; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block three, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
In this example, the melt index of polypropylene is 3 g/10min, the temperature of the three zones from the front to the back of the feeding section 4 is 100.0 ℃, 110.0 ℃ and 120.0 ℃, the temperature of the six zones from the front to the back of the plasticizing section 5 is 200.0 ℃, 250.0 ℃, 200.0 ℃, the injection pressure of industrial oxygen is 0.5MPa, the temperature of the two zones from the front to the back of the exhaust section 6 is 180.0 ℃, 160.0 ℃, the temperature of the metering section 7 is 150 ℃, and the polypropylene formed by extrusion is prepared by: 20 g/10 min.

Claims (5)

1. A method for preparing polypropylene resin with large melt index is characterized in that: the method comprises the following steps: step 1, feeding polypropylene particles into a feeding section (4) of a co-rotating twin-screw extruder through a feeding port (1), wherein the temperature of the feeding section is 100-120 ℃, and under the action of a forward conveying block and a feeding section shearing block of the feeding section, the polypropylene particles are heated, compressed and fed to a plasticizing section (5) forward; step 2, injecting industrial oxygen with the pressure of 0.1-1.0 Mpa into a gas injection port (2) of the plasticizing section, fully contacting and mixing the molten polypropylene and the industrial oxygen at the temperature of 180-280 ℃, degrading the molten polypropylene under the action of a shearing block of the plasticizing section and a reverse conveying block of the plasticizing section, and conveying the degraded polypropylene to a gas exhaust section (6); step 3, discharging residual oxygen from the exhaust port (3) under the action of the exhaust section shearing block, the exhaust section reverse conveying block and the exhaust section forward conveying block at the temperature of 160-180 ℃, and conveying degraded polypropylene to the metering section (7); and 4, extruding the degraded polypropylene into strips from a machine head and a mouth die at the temperature of 140-160 ℃ under the action of a forward conveying block of the metering section, cooling by a water tank, pelletizing and drying to form large melt index polypropylene particles.
2. The method for preparing a large melt index polypropylene resin according to claim 1, wherein: the diameter of a screw of the co-rotating double-screw extruder is 20 mm-120 mm, and the length-diameter ratio is 28-52.
3. The method for preparing a large melt index polypropylene resin according to claim 1, wherein: the melt index of the polypropylene particles is 2-100 g/10min, and the melt index of the large melt index polypropylene particles after extrusion granulation is 15-2500 g/10 min.
4. The method for preparing a large melt index polypropylene resin according to claim 1, wherein: the feeding section forward conveying block and the feeding section shearing block comprise a 48mm forward conveying block I, a 64mm forward conveying block I, 3 48mm forward conveying blocks II, a 64mm forward conveying block II, 2 48mm forward conveying blocks III, a 30-degree shearing block I and a 45-degree shearing block I which are arranged from front to back; the plasticizing section shear block and the plasticizing section reverse conveying block comprise a first 60-degree shear block, a first 90-degree shear block, a first 32-mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a second 32-mm reverse conveying block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a third 32-mm reverse conveying block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a fourth 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block, a fifth 32-mm reverse conveying block and a sixth 30-degree shear block; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block six, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
5. The method for preparing a large melt index polypropylene resin according to claim 1, wherein: the feeding section forward conveying block and the feeding section shearing block comprise a 48mm forward conveying block I, a 64mm forward conveying block I, 3 48mm forward conveying blocks II, a 64mm forward conveying block II, 3 48mm forward conveying blocks III and a 30-degree shearing block I which are arranged from front to back; the plasticizing section shear block and the plasticizing section reverse conveying block comprise a first 45-degree shear block, a first 60-degree shear block, a first 90-degree shear block, a first 32mm reverse conveying block, a second 30-degree shear block, a second 45-degree shear block, a second 60-degree shear block, a second 90-degree shear block, a third 30-degree shear block, a third 45-degree shear block, a third 60-degree shear block, a third 90-degree shear block, a fourth 30-degree shear block, a fourth 45-degree shear block, a fourth 60-degree shear block, a fourth 90-degree shear block, a second 32-mm reverse conveying block, a fifth 30-degree shear block, a fifth 45-degree shear block, a fifth 60-degree shear block, a fifth 90-degree shear block and a sixth 30-degree shear block which are arranged from front to back; the exhaust section shear block, the exhaust section reverse conveying block and the exhaust section forward conveying block comprise a 45-degree shear block six, a 90-degree shear block six, a 32-mm reverse conveying block three, 3 64-mm forward conveying blocks three and a 48-mm forward conveying block four which are arranged from front to back; the metering section forward conveying blocks comprise 2 32mm forward conveying blocks and 4 24mm forward conveying blocks which are arranged from front to back.
CN202010310091.4A 2020-04-20 2020-04-20 Method for preparing polypropylene resin with large melt index Pending CN111333754A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115505168A (en) * 2021-06-23 2022-12-23 松山湖材料实验室 Production of high-fluidity polypropylene by chemical degradation method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3551943A (en) * 1966-12-19 1971-01-05 Exxon Research Engineering Co Controlled degradation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3551943A (en) * 1966-12-19 1971-01-05 Exxon Research Engineering Co Controlled degradation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115505168A (en) * 2021-06-23 2022-12-23 松山湖材料实验室 Production of high-fluidity polypropylene by chemical degradation method
CN115505168B (en) * 2021-06-23 2024-03-08 松山湖材料实验室 Production of high fluidity polypropylene by chemical degradation method

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