CN107513132A - A kind of high melt strength polypropylene material and preparation method thereof - Google Patents
A kind of high melt strength polypropylene material and preparation method thereof Download PDFInfo
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- CN107513132A CN107513132A CN201710877421.6A CN201710877421A CN107513132A CN 107513132 A CN107513132 A CN 107513132A CN 201710877421 A CN201710877421 A CN 201710877421A CN 107513132 A CN107513132 A CN 107513132A
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- melt strength
- parts
- high melt
- benzoyl peroxide
- polypropylene material
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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
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- 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
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/06—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92514—Pressure
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
-
- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
Abstract
The invention discloses a kind of high melt strength polypropylene material and preparation method thereof, high melt strength polypropylene material of the present invention, the component comprising following parts by weight is prepared by the grafting of extruder extrusion reaction：100 parts of acrylic resin, 14 parts of crosslinking agent, benzoyl peroxide paste 0.1 1 parts, and 0.1 1.5 parts of antioxidant, the melt index of described acrylic resin is 6 15g/10min, and the mass content of benzoyl peroxide is 50% 55% in benzoyl peroxide paste.The preparation method of high melt strength polypropylene material of the present invention uses three screw rod cocurrent and parallel rotary extrusion machines.Its melt strength of high melt strength polypropylene material produced by the invention is 1.5 15 times of its key component acrylic resin, heat-resist, strain hardening effect, mechanical performance are excellent, control structure according to demand, it can be widely used in the fields such as polypropylene expanded and thermoforming.
Description
Technical field
The present invention relates to a kind of polypropylene material and preparation method thereof, more particularly to a kind of high melt strength polypropylene material
And preparation method thereof.
Background technology
Polypropylene (PP) is one of as five big general thermoplastic resins, not only abundant raw material, cheap, also with fusing point
Height, excellent heat resistance, mechanical performance are excellent and the features such as being easy to processing and forming, in transport (automobile interior trim and bumper bar), hard
Pack (bottle cap, pallet, Turnover Box etc.), apparatus and medical product (syringe, tool box etc.), human food snack box, industrial or agricultural and
The fields such as daily necessities all obtain universal application.
Because plain polypropylene softening point is close to melting temperature, PP melt strength (melt viscosity) meeting when causing to process
Drastically decline, be suitable for that the temperature range of processing is narrow, and chamber wall thickness is uneven when easily causing thermoforming during extrusion foaming, does not have
Significant strain hardening effect, the problems such as abscess collapses during foaming.Improving the polypropylene after melt strength of polypropylene has significantly
Strain hardening behavior, higher melt strength is shown within the scope of temperature that can be wider and is connect to stretch viscosity, to extrusion foaming,
The processing technologys such as high-speed coating, melt spinning are favourable, and the branched structure of high melt strength, propylene (HMSPP) is common PP
1.5-15 times, gel content is low, and processability is good, recoverable, HMSPP as in general-purpose plastics PP important modification kind,
It is developed and characterized and is paid close attention to by domestic and international researcher in recent years.
Improving polyacrylic melt strength typically has the methods of chemical crosslinking, cross-linking radiation, reactive grafting and blending and modifying.
Chemical crosslinking is that peroxide is added in polypropylene, and heat resolve produces free radical, triggers the crosslinking of polypropylene molecular chain anti-
Should, due to molecular structure, β fractures easily occur during chemical crosslinking for polypropylene, finally result in material degradation.
Chinese Academy of Sciences's chemistry once used DCP to trigger unsaturated silane grafting, prepared HMSPP, but same in higher DCP and silane contents
When it is existing under the conditions of could obtain gel, while the product being chemically crosslinked has unpleasant peculiar smell, limits application.
Chinese patent CN1142514A reports Beijing Chemical Research Institute and Peking University passes through60Gamma-rays spoke caused by Co
Penetrate polypropylene and prepare high melt strength, propylene, be characterized in adding a certain amount of nucleator in polypropylene, it is existing to overcome
The shortcomings that mechanical property is not obviously improved under degradation of polypropylene and normal temperature during crosslinking with radiation present in technology.Polypropylene
Radiation modification generally requires vacuum or nitrogen protection, and to reduce the oxidative degradation in radiative process, processing environment is to industry
Metaplasia production brings very big obstruction.
The content of the invention
The technical problem to be solved in the present invention is：The present invention provides a kind of high melt strength polypropylene material, and provides
A kind of preparation method that high melt strength polypropylene material is prepared with extrusion reaction Graft Method.
In order to solve the above-mentioned technical problem, high melt strength polypropylene material of the present invention, the component of following parts by weight is included
It is prepared by the grafting of extruder extrusion reaction：
The melt index of described acrylic resin is 6-15g/10min, benzoyl peroxide in the benzoyl peroxide paste
The mass content of formyl is 50%-55%.
Preferably, described crosslinking agent is selected from trifunctional group acrylate, pentaerythritol triacrylate, trihydroxy methyl third
Alkane triacrylate, ethoxylated trimethylolpropane 3 third wish one or more mixtures in acid esters.
Preferably, described crosslinking agent is trimethylolpropane trimethacrylate.
Preferably, described crosslinking agent is that ethoxylated trimethylolpropane 3 third wishes acid esters.
The preparation method of high melt strength polypropylene material of the present invention, described high melt strength polypropylene material include such as
The component of lower parts by weight is prepared by the grafting of extruder extrusion reaction：
The melt index of described acrylic resin is 6-15g/10min, benzoyl peroxide in the benzoyl peroxide paste
The mass content of formyl is 50%-55%, and described crosslinking agent is selected from trifunctional group acrylate, the acrylic acid of pentaerythrite three
Ester, trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane 3 third wish one or more mixing in acid esters
Thing, described extruder refer to three screw rod cocurrent and parallel rotary extrusion machines, and its three screw rods are arranged in parallel, and the axis of three screw rods exists
In same plane.
Preferably, the preparation method of high melt strength polypropylene material of the present invention comprises the following steps：
(1) acrylic resin, crosslinking agent, benzoyl peroxide paste, antioxidant are taken；
(2) acrylic resin, benzoyl peroxide paste, antioxidant whole component are sequentially added in high mixer with 450
After rev/min speed mixing 5min, addition crosslinking agent remixes 10min under conditions of not speed change is not shut down；Mixed process
Temperature of charge in middle high mixer is controlled at 40-60 DEG C；
(3) material mixed is extruded through three screw rod cocurrent and parallel rotary extrusion machines, extrusion of the material in extruder
It is crosslinked in journey, graft reaction, is made high melt strength polypropylene material, three screw rod cocurrent and parallel rotary extrusion machines is from feeding
Mouth is disposed with nine heating zones and heating head to discharging opening, and being provided with hydraulic pressure between the 9th heating zone and heating head changes
Wire stitcher area, is provided with filter plate in hydraulic screen replacing device, on filter plate plus puts stainless steel filtering net during extrusion so that stainless steel filtering net can be with
Change, three screw rods be arranged in parallel, and in the same plane, three screw rods run through nine heating zones to the axis of three screw rods, discharging
Mouthful it is arranged on head, three screw rods rotate in same direction during operating, and stainless steel filtering net includes two layers of 40 mesh stainless steel filtering nets, extruder
Nine Heating Zone Temperatures be set as successively 130 DEG C, 135 DEG C, 135 DEG C, 140 DEG C, 155 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190
DEG C, 200 DEG C of hydraulic screen replacing device temperature, 190 DEG C of head temperature, change a stainless steel filtering net, three spiral shells within every four hours during production
The rev/min of rotating speed 200 of bar, the vacuum in extruder are maintained in the range of -0.08Mpa to -0.1Mpa.
The beneficial effects of the invention are as follows：The present invention adds crosslinking agent in a kind of acrylic resin, benzoyl peroxide is pasted,
Antioxidant, it is compounded through three screw rod rotating Vortex extruders, by being crosslinked in three screw rod rotating Vortex extruders and branched anti-
Should, obtain high melt strength polypropylene material.This method is to processing environment and process equipment, technique without rigors, simple nothing
Pollution, is a kind of Perfected process of industrialized production high melt strength polypropylene material.The high melt strength, propylene material of production
It is 1.5-15 times of its key component acrylic resin to expect its melt strength, and heat-resist, strain hardening effect, mechanical performance are excellent
Different, control structure, can be widely used in the fields such as polypropylene expanded and thermoforming according to demand.
The present invention adds crosslinking agent in acrylic resin, is pasted with benzoyl peroxide and triggers crosslinking agent, same in three screw rods
Extrusion crosslinking, graft reaction into rotary extrusion machine, and three screw rod rotating Vortex extruder flow fields are complicated, the residence time is long, mixed
Refining performance is good, and molecule in flow process, can be also grafted by material in three screw rod rotating Vortex extruders, can be preferable
The structure of high melt strength, propylene is controlled, to be respectively applied to the different processing technologys such as polypropylene expanded and thermoforming, to height
Melt strength polypropylene has opened up broader practice field.
Embodiment
The present invention is prepared by the following method high melt strength polypropylene material：
(1) acrylic resin, crosslinking agent, benzoyl peroxide paste, antioxidant are taken；Benzoyl peroxide paste is peroxidating
Benzoyl is stirred to pasty state with silicone oil and is made, and benzoyl peroxide mass content is 50-55% in benzoyl peroxide paste, antioxygen
Agent can use four { β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid } pentaerythritol esters.
(2) acrylic resin, benzoyl peroxide paste, antioxidant whole component are sequentially added in high mixer with 450
After rev/min speed mixing 5min, addition crosslinking agent remixes 10min under conditions of not speed change is not shut down；Mixed process
Temperature of charge in middle high mixer is controlled at 40-60 DEG C；
(3) material mixed is extruded through three screw rod cocurrent and parallel rotary extrusion machines, extrusion of the material in extruder
It is crosslinked in journey, graft reaction, is made high melt strength polypropylene material, three screw rod cocurrent and parallel rotary extrusion machines is from feeding
Mouth is disposed with nine heating zones and heating head to discharging opening, and being provided with hydraulic pressure between the 9th heating zone and heating head changes
Wire stitcher area, is provided with filter plate in hydraulic screen replacing device, and stainless steel filtering net is set on filter plate during extrusion so that stainless steel filtering net can be with
Change, three screw rods be arranged in parallel, and in the same plane, three screw rods run through nine heating zones to the axis of three screw rods, discharging
Mouth is arranged on head.Three screw rods rotate in same direction during operating.Stainless steel filtering net includes two layers of 40 mesh stainless steel filtering nets.Extruder
Nine Heating Zone Temperatures be set as successively 130 DEG C, 135 DEG C, 135 DEG C, 140 DEG C, 155 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190
DEG C, 200 DEG C of hydraulic screen replacing device temperature, 190 DEG C of head temperature, change a stainless steel filtering net, three spiral shells within every four hours during production
The rev/min of rotating speed 200 of bar, the 8th heating zone are connected with vavuum pump, the vacuum in extruder be maintained at -0.08Mpa to -
In the range of 0.1Mpa.
Of the invention specific to implement following groups embodiment as stated above, the component and content of every group of embodiment are shown in Table 1,
The high melt strength polypropylene material performance that every group of embodiment obtains is shown in Table 2.
Melt index determination using GB-T 3682-2000 thermoplastics melt mass flow rates and melts in the present invention
The measure of body rate of volume flow, test condition：Nominal load 2.16KG, 230 DEG C of test temperature.The polypropylene that the present invention uses
Resin melt strength：2.5-2.6cN.
Table 1
Table 2
Claims (6)
1. a kind of high melt strength polypropylene material, the component comprising following parts by weight is grafted by extruder extrusion reaction and prepared
Form：
100 parts of acrylic resin,
Crosslinking agent 1-4 parts,
Benzoyl peroxide pastes 0.1-1 parts,
0.1-1.5 parts of antioxidant,
The melt index of described acrylic resin is 6-15g/10min, benzoyl peroxide in the benzoyl peroxide paste
Mass content be 50%-55%.
2. high melt strength polypropylene material according to claim 1, it is characterised in that：Described crosslinking agent is selected from three officials
Acrylate, pentaerythritol triacrylate, trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane three can be rolled into a ball
One or more mixtures in third uncommon acid esters.
3. high melt strength polypropylene material according to claim 1, it is characterised in that：Described crosslinking agent is three hydroxyl first
Base propane triacrylate.
4. high melt strength polypropylene material according to claim 1, it is characterised in that：Described crosslinking agent is ethyoxyl
Change trimethylolpropane tris third and wish acid esters.
A kind of 5. preparation method of high melt strength polypropylene material, it is characterised in that：Described high melt strength, propylene material
Component of the material comprising following parts by weight is prepared by the grafting of extruder extrusion reaction：
100 parts of acrylic resin,
Crosslinking agent 1-4 parts,
Benzoyl peroxide pastes 0.1-1 parts,
0.1-1.5 parts of antioxidant,
The melt index of described acrylic resin is 6-15g/10min, benzoyl peroxide in the benzoyl peroxide paste
Mass content be 50%-55%, described crosslinking agent is selected from trifunctional group acrylate, pentaerythritol triacrylate, three hydroxyls
Propane tri, ethoxylated trimethylolpropane 3 third wish one or more mixtures in acid esters, described
Extruder refer to three screw rod cocurrent and parallel rotary extrusion machines, its three screw rods are arranged in parallel, and the axis of three screw rods is same flat
In face.
6. the preparation method of high melt strength polypropylene material according to claim 5, it is characterised in that：The preparation side
Method comprises the following steps：
（1）Take acrylic resin, crosslinking agent, benzoyl peroxide paste, antioxidant；
（2）By acrylic resin, benzoyl peroxide paste, antioxidant whole component sequentially add in high mixer with 450 turns/it is every
After minute speed mixing 5min, addition crosslinking agent remixes 10min under conditions of not speed change is not shut down；It is high mixed in mixed process
Temperature of charge in machine is controlled at 40-60 DEG C；
（3）The material mixed is extruded through three screw rod cocurrent and parallel rotary extrusion machines, material is in the extrusion of extruder
Be crosslinked, connect by-reaction, be made high melt strength polypropylene material, three screw rod cocurrent and parallel rotary extrusion machines from spout to
Discharging opening is disposed with nine heating zones and heating head, and hydraulic screen replacing device is provided between the 9th heating zone and heating head
Area, is provided with filter plate in hydraulic screen replacing device, on filter plate plus puts stainless steel filtering net during extrusion so that stainless steel filtering net can be more
Change, three screw rods be arranged in parallel, and in the same plane, three screw rods run through nine heating zones, discharging opening to the axis of three screw rods
It is arranged on head, three screw rods rotate in same direction during operating, and stainless steel filtering net includes two layers of 40 mesh stainless steel filtering nets, extruder
Nine Heating Zone Temperatures be set as successively 130 DEG C, 135 DEG C, 135 DEG C, 140 DEG C, 155 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190
DEG C, 200 DEG C of hydraulic screen replacing device temperature, 190 DEG C of head temperature, change a stainless steel filtering net, three spiral shells within every four hours during production
The rev/min of rotating speed 200 of bar, the vacuum in extruder are maintained in the range of -0.08Mpa to -0.1Mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710877421.6A CN107513132A (en) | 2017-09-26 | 2017-09-26 | A kind of high melt strength polypropylene material and preparation method thereof |
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| CN201710877421.6A CN107513132A (en) | 2017-09-26 | 2017-09-26 | A kind of high melt strength polypropylene material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553724A (en) * | 2018-11-28 | 2019-04-02 | 山东玉皇化工有限公司 | A kind of high melt strength polypropylene material and preparation method thereof |
| CN112940153A (en) * | 2021-05-06 | 2021-06-11 | 上海圆暖高分子材料科技有限公司 | Method for grafting modified polar monomer through high-molecular polymer reaction extrusion |
| CN113637260A (en) * | 2021-09-10 | 2021-11-12 | 河南大张过滤技术研究院有限公司 | Modified polypropylene composite material filter plate of filter press and continuous preparation method thereof |
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| CN102558449A (en) * | 2011-12-13 | 2012-07-11 | 金发科技股份有限公司 | High-melt-strength polypropylene material, and preparation method and application thereof |
| CN103865176A (en) * | 2012-12-10 | 2014-06-18 | 中国石油天然气股份有限公司 | Preparation method of high-melt-strength polypropylene |
| CN104356305A (en) * | 2014-10-30 | 2015-02-18 | 徐州工业职业技术学院 | Method for preparing high-melt-strength polypropylene based on solid phase grafting |
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2017
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| CN1986589A (en) * | 2006-12-15 | 2007-06-27 | 中国科学院长春应用化学研究所 | Polypropylene resin with high melt strength and its preparing method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553724A (en) * | 2018-11-28 | 2019-04-02 | 山东玉皇化工有限公司 | A kind of high melt strength polypropylene material and preparation method thereof |
| CN112940153A (en) * | 2021-05-06 | 2021-06-11 | 上海圆暖高分子材料科技有限公司 | Method for grafting modified polar monomer through high-molecular polymer reaction extrusion |
| CN113637260A (en) * | 2021-09-10 | 2021-11-12 | 河南大张过滤技术研究院有限公司 | Modified polypropylene composite material filter plate of filter press and continuous preparation method thereof |
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