CN110079019A - A kind of PA-PP hybrid resin material of toughening modifying and preparation method thereof - Google Patents
A kind of PA-PP hybrid resin material of toughening modifying and preparation method thereof Download PDFInfo
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- CN110079019A CN110079019A CN201910424964.1A CN201910424964A CN110079019A CN 110079019 A CN110079019 A CN 110079019A CN 201910424964 A CN201910424964 A CN 201910424964A CN 110079019 A CN110079019 A CN 110079019A
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- montmorillonite
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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
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
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Abstract
The present invention discloses a kind of PA-PP hybrid resin material and preparation method thereof of toughening modifying, processing is modified to montmorillonite surface with rare-earth coupling agent, the montmorillonite after modification is introduced in polypropylene fusion graft maleic anhydride using melt grafting later, finally by maleic anhydride inoculated polypropylene/modified montmorillonoid master batch, it is rare earth modified after montmorillonite be added in the melt blending system of polypropylene and nylon, obtain hybrid resin material.Montmorillonite after rare-earth coupling agent modification has induction beta crystal heterogeneous nucleating effect, effectively facilitates the conversion of crystal form in PP matrix, help to improve the knot toughness of composite material；Montmorillonite after modification is introduced into the graft reaction of polypropylene and maleic anhydride, helps to improve grafting rate, improved the compatibility of both polypropylene and nylon, realize effective increase-volume.
Description
Technical field
The present invention relates to technical field of polymer, and in particular to a kind of PA-PP hybrid resin material of toughening modifying and its
Preparation method.
Background technique
The features such as polypropylene (PP) resin has processing performance good, and chemical-resistance is good, and water absorption resistance can be excellent, but simultaneously
It is low with room temperature notch impact strength, the disadvantages of poor heat resistance and poor dimensional stability, thus limit its scope of application.Make
For important engineering plastics, nylon (PA) has excellent mechanical property, heat resistance, wearability and high rigidity, but the thermal change of PA6
Shape temperature is lower, easy to moisture absorption, and dimensional stability is poor, to limit further applying for PA6.PP/PA alloy system is ground
Studying carefully main purpose is that realization is blended by PA and PP to be mutually modified, and is learnt from other's strong points to offset one's weaknesses.However, PP belongs to non-polar polymer, PA belongs to
In polar polymer, the two different polarities are very big, and it is poor that gained alloy property is directly blended.
In recent years, organic modification montmonrillonite (OMMT) is widely used in the modification of blend polymer.Khatua etc.
People has found in PA6/ EP rubbers (PA6/EPR) blend that OMMT is selectively scattered in PA6, can effectively prevent dispersed phase EPR
It is poly- simultaneously, to reduce the phase size of EPR.Li Yongjin et al. has found that in PA6/PPO blend, OMMT can reduce dispersed phase
The phase size of PPO.But lamella parent's polarity of montmorillonite, nonpolar molecule are difficult the piece interlayer that intercalation enters montmorillonite, molten
Melt during blending method prepares level polypropylene/montmorillonoid composite material, can all select compatilizer generally to improve polypropylene and cover
The compatibility of soil is taken off, the compatilizer usually selected is polypropylene grafted maleic anhydride.
Summary of the invention
To solve above-mentioned the deficiencies in the prior art, the present invention proposes a kind of PA-PP hybrid resin of toughening modifying
Material and preparation method thereof improves the compatibility of polypropylene and nylon resin, improves the mechanical property and heat resistance of composite material
Energy.
To realize the above-mentioned technical purpose, the invention discloses a kind of preparations of the PA-PP hybrid resin material of toughening modifying
Method is modified processing to montmorillonite surface with rare-earth coupling agent, later using melt grafting in polypropylene fusion graft
The montmorillonite after modification is introduced in maleic anhydride, finally by maleic anhydride inoculated polypropylene/modified montmorillonoid master batch, rare earth
Modified montmorillonite is added in the melt blending system of polypropylene and nylon, obtains hybrid resin material.
Further, in the maleic anhydride inoculated polypropylene/modified montmorillonoid master batch montmorillonite content in 6-15%.
Further, in the rare-earth coupling agent modified montmorillonoid usage amount of rare-earth coupling agent in 1.0-5.0%.
It is specific the preparation method is as follows:
(1) preparation of rare-earth coupling agent modified montmorillonoid: being placed in 110-130 DEG C of baking oven dry 6-10h for montmorillonite, cold
But 200-300 mesh is crossed to grinding at room temperature, placed it in high-speed mixer, control revolving speed is that 600-1000r/min stirs 15-
30min rises to 80-90 DEG C to temperature, keeps temperature-resistant, several times a small amount of addition rare-earth coupling agent, between each feed time
It is interposed between 10-15min, charging process keeps high-speed stirred, continues to stir 10-20min after the completion of charging, is cooled to room temperature, discharges；
(2) according to montmorillonite/DCP (6-12): 1 mass ratio weighs appropriate DCP and is dissolved in solvent, by DCP solution and portion
The rare-earth coupling agent modified montmorillonoid of (1) preparation is added in above-mentioned high-speed mixer step by step, is stirred to solvent and is volatilized
Completely；
(3) be (2-4) according to montmorillonite/maleic anhydride: maleic anhydride is added to step (2) mixture 1 mass ratio
In material, acrylic resin is added after mixing later, co-extrusion, pelletizing are melted using double screw extruder, screw speed is in 40-
60r/min, the temperature of extruder are 210-230 DEG C, obtain maleic anhydride inoculated polypropylene/modified montmorillonoid master batch；
(4) by a certain proportion of polypropylene, nylon, expanding material under the conditions of 230-250 DEG C melting mixing 8-15min, it
After be cooled to 190-210 DEG C, be added above-mentioned preparation maleic anhydride inoculated polypropylene/modified montmorillonoid master batch, with step (1) make
Standby rare-earth coupling agent modified montmorillonoid continues extruding pelletization after mixing 5-15min, PA-PP hybrid resin material is made.
Further, one of solvent selection acetone, ethyl alcohol, ether, acetic acid or petroleum ether in the step (2).
The invention also discloses a kind of PA-PP hybrid resin materials of toughening modifying being prepared such as above-mentioned preparation method
Material, the PA-PP hybrid resin material include the acrylic resin of 100 parts by weight, 30-45 parts of nylon, 4-8 parts of expanding materials,
8-15 parts of maleic anhydride inoculated polypropylenes/modified montmorillonoid master batch, 4-9 parts of rare-earth coupling agent modified montmorillonoids.
Compared with the prior art, the invention has the following advantages:
(1) present invention is modified processing to montmorillonite using rare-earth coupling agent, and montmorillonite surface parent not only can be improved
Hydrophobic performance improves the compatibility between montmorillonite and acrylic resin, while the illiteracy after rare-earth coupling agent modification is de-
Soil has induction beta crystal heterogeneous nucleating effect, effectively facilitates the conversion of crystal form in PP matrix, help to improve composite material
Tie toughness.
(2) montmorillonite after modification is introduced into the graft reaction of polypropylene and maleic anhydride, helps to improve and connects
Branch rate, maleic anhydride inoculated polypropylene/modified montmorillonoid master batch of generation play the role of expanding material, and anhydride group can be with nylon
It reacts and generates PP-g-PA, so that interfacial tension be effectively reduced, improve the compatibility of both polypropylene and nylon, realization has
Imitate increase-volume.
(3) during the melt blending of polypropylene and nylon, after preliminary cooling, nylon crystallization, and polypropylene is in molten
Melt state, the montmorillonite modified containing rare-earth coupling agent be added at this time, helps to be dispersed in the polypropylene of molten condition,
Promote the generation of β crystal in polypropylene, improves β crystalline content in composite material, achieve the purpose that toughening modifying.
Specific embodiment
Embodiment 1
A kind of PA-PP hybrid resin material of toughening modifying, the preparation method is as follows:
(1) preparation of rare-earth coupling agent modified montmorillonoid: montmorillonite is placed in 120 DEG C of baking ovens dry 8h, is cooled to room
The ground 200-300 mesh of temperature, places it in high-speed mixer, and control revolving speed is that 800r/min stirs 20min, to temperature liter
It to 85 DEG C, keeps temperature-resistant, rare-earth coupling agent is added on a small quantity several times, each feed time is spaced in 10min, and feed process
High-speed stirred is kept, continues to stir 15min after the completion of charging, is cooled to room temperature, discharge；
The usage amount of the rare-earth coupling agent is 2.5%.
(2) according to montmorillonite/DCP be 10:1 mass ratio, weigh appropriate DCP and be dissolved in acetone, by DCP acetone soln with
The rare-earth coupling agent modified montmorillonoid of part steps (1) preparation is added in above-mentioned high-speed mixer, is stirred to acetone and is waved
It distributes complete；
(3) mass ratio for being 3: 1 according to montmorillonite/maleic anhydride, maleic anhydride is added to step (2) mixed material
In, acrylic resin is added after mixing later, co-extrusion, pelletizing are melted using double screw extruder, screw speed is in 60r/
Min, the temperature of extruder are 220 DEG C, obtain maleic anhydride inoculated polypropylene/modified montmorillonoid master batch；
Montmorillonite content is 10% in the maleic anhydride inoculated polypropylene/modified montmorillonoid master batch.
(4) it by 100 parts of polypropylene, 40 parts of nylon, 4 parts of expanding materials melting mixing 10min under the conditions of 235 DEG C, drops later
Temperature is added maleic anhydride inoculated polypropylene/modified montmorillonoid master batch of 12 parts of above-mentioned preparations, makes with 5 parts of steps (1) to 195 DEG C
Standby rare-earth coupling agent modified montmorillonoid continues extruding pelletization after mixing 10min, PA-PP hybrid resin material is made.
Embodiment 2
A kind of PA-PP hybrid resin material of toughening modifying, the preparation method is as follows:
(1) preparation of rare-earth coupling agent modified montmorillonoid: montmorillonite is placed in 120 DEG C of baking ovens dry 8h, is cooled to room
The ground 200-300 mesh of temperature, places it in high-speed mixer, and control revolving speed is that 800r/min stirs 20min, to temperature liter
It to 85 DEG C, keeps temperature-resistant, rare-earth coupling agent is added on a small quantity several times, each feed time is spaced in 10min, and feed process
High-speed stirred is kept, continues to stir 15min after the completion of charging, is cooled to room temperature, discharge；
The usage amount of the rare-earth coupling agent is 2.5%.
(2) according to montmorillonite/DCP be 10:1 mass ratio, weigh appropriate DCP and be dissolved in acetone, by DCP acetone soln with
The rare-earth coupling agent modified montmorillonoid of part steps (1) preparation is added in above-mentioned high-speed mixer, is stirred to acetone and is waved
It distributes complete；
(3) mass ratio for being 3: 1 according to montmorillonite/maleic anhydride, maleic anhydride is added to step (2) mixed material
In, acrylic resin is added after mixing later, co-extrusion, pelletizing are melted using double screw extruder, screw speed is in 60r/
Min, the temperature of extruder are 220 DEG C, obtain maleic anhydride inoculated polypropylene/modified montmorillonoid master batch；
Montmorillonite content is 10% in the maleic anhydride inoculated polypropylene/modified montmorillonoid master batch.
(4) it by 100 parts of polypropylene, 40 parts of nylon, 4 parts of expanding materials melting mixing 10min under the conditions of 235 DEG C, drops later
Temperature is added maleic anhydride inoculated polypropylene/modified montmorillonoid master batch of 9 parts of above-mentioned preparations, prepares with 7 parts of steps (1) to 195 DEG C
Rare-earth coupling agent modified montmorillonoid, continue be kneaded 10min after extruding pelletization, be made PA-PP hybrid resin material.
Embodiment 3
Raw material components are same as Example 1, difference from example 1 is that, step (2) polypropylene in embodiment 3
With modified montmorillonite is not added in the graft reaction of maleic anhydride, and be directly added in step (4), preparation is modified
PA-PP material.
Embodiment 4
Raw material components are same as Example 2, with embodiment 2 the difference is that, step (2) polypropylene in embodiment 4
With modified montmorillonite is not added in the graft reaction of maleic anhydride, and be directly added in step (4), preparation is modified
PA-PP material.
Embodiment 5
Respectively according to the specific preparation method of embodiment 1, embodiment 2, embodiment 3 and embodiment 4,4 groups are respectively obtained
The modified PA-PP resin mixed material of difference, and carry out corresponding performance detection.
Tensile strength presses ASTM D-638 standard, and bending strength presses ASTM D-790 standard, carries out sample preparation test.Impact is strong
Degree test: according to GB/T 1843-1996, using the impact strength of balance weight impact testing machine measurement sample.Test result is shown in Table
1。
The test result of the modified PA-PP material of table 1
| Sample | Stretching yield stress/MPa | Bending modulus/MPa | Impact strength (J/m) |
| Pure PP | 21.6 | 965 | 46 |
| Embodiment 1 | 23.9 | 1027 | 84 |
| Embodiment 2 | 24.1 | 1031 | 86 |
| Embodiment 3 | 23.2 | 1005 | 75 |
| Embodiment 4 | 22.8 | 997 | 73 |
As seen from the above table: in the identical situation of each component content, using embodiment 1, the modification of 2 method of embodiment preparation
PA-PP material property is better than 3,4 two groups of materials of embodiment, it is known that, the montmorillonite after modification is introduced into polypropylene and horse
Come in the graft reaction of acid anhydrides, help to improve grafting rate, so that montmorillonite, polypropylene is mixed and is uniformly dispersed with nylon three, mention
The compatibility of both high polypropylene and nylon helps to improve the growth of PP crystal, improves the mechanical property of PA-PP material.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (6)
1. a kind of preparation method of the PA-PP hybrid resin material of toughening modifying, which is characterized in that de- to covering with rare-earth coupling agent
Native surface is modified processing, after introducing modification in polypropylene fusion graft maleic anhydride using melt grafting later
Montmorillonite, finally by maleic anhydride inoculated polypropylene/modified montmorillonoid master batch, it is rare earth modified after montmorillonite be added to poly- third
In the melt blending system of alkene and nylon, hybrid resin material is obtained.
2. a kind of preparation method of the PA-PP hybrid resin material of toughening modifying according to claim 1, feature exist
In montmorillonite content is in 6-15% in the maleic anhydride inoculated polypropylene/modified montmorillonoid master batch.
3. a kind of preparation method of the PA-PP hybrid resin material of toughening modifying according to claim 1, feature exist
In the usage amount of rare-earth coupling agent is in 1.0-5.0% in the rare-earth coupling agent modified montmorillonoid.
4. the preparation method of the PA-PP hybrid resin material of -3 any a kind of toughening modifyings according to claim 1, special
Sign is, it is specific the preparation method is as follows:
(1) preparation of rare-earth coupling agent modified montmorillonoid: montmorillonite is placed in 110-130 DEG C of baking oven dry 6-10h, is cooled to
Grinding at room temperature crosses 200-300 mesh, places it in high-speed mixer, and control revolving speed is that 600-1000r/min stirs 15-
30min rises to 80-90 DEG C to temperature, keeps temperature-resistant, several times a small amount of addition rare-earth coupling agent, between each feed time
It is interposed between 10-15min, charging process keeps high-speed stirred, continues to stir 10-20min after the completion of charging, is cooled to room temperature, discharges；
(2) according to montmorillonite/DCP (6-12): 1 mass ratio weighs appropriate DCP and is dissolved in solvent, and DCP solution and part are walked
Suddenly the rare-earth coupling agent modified montmorillonoid of (1) preparation is added in above-mentioned high-speed mixer, is stirred complete to solvent volatilization；
(3) be (2-4) according to montmorillonite/maleic anhydride: maleic anhydride is added to step (2) mixed material 1 mass ratio
In, acrylic resin is added after mixing later, co-extrusion, pelletizing are melted using double screw extruder, screw speed is in 40-
60r/min, the temperature of extruder are 210-230 DEG C, obtain maleic anhydride inoculated polypropylene/modified montmorillonoid master batch；
(4) by a certain proportion of polypropylene, nylon, expanding material under the conditions of 230-250 DEG C melting mixing 8-15min, drop later
Temperature to 190-210 DEG C, be added above-mentioned preparation maleic anhydride inoculated polypropylene/modified montmorillonoid master batch, with step (1) preparation
Rare-earth coupling agent modified montmorillonoid continues extruding pelletization after mixing 5-15min, PA-PP hybrid resin material is made.
5. a kind of preparation method of the PA-PP hybrid resin material of toughening modifying according to claim 4, feature exist
In one of solvent selection acetone, ethyl alcohol, ether, acetic acid or petroleum ether in the step (2).
6. a kind of PA-PP hybrid resin material of toughening modifying that preparation method as claimed in claim 4 obtains, feature exist
In, the PA-PP hybrid resin material include the acrylic resin of 100 parts by weight, 30-45 parts of nylon, 4-8 parts of expanding materials,
8-15 parts of maleic anhydride inoculated polypropylenes/modified montmorillonoid master batch, 4-9 parts of rare-earth coupling agent modified montmorillonoids.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982253A (en) * | 2019-12-24 | 2020-04-10 | 上海中镭新材料科技有限公司 | Polyamide material and preparation method and application thereof |
| CN111019339A (en) * | 2019-12-24 | 2020-04-17 | 上海中镭新材料科技有限公司 | Spraying-free metallic polyamide material and preparation method and application thereof |
| CN115340728A (en) * | 2022-09-15 | 2022-11-15 | 广东锦湖日丽高分子材料有限公司 | Scratch-resistant polypropylene resin material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115340728B (en) * | 2022-09-15 | 2023-08-01 | 广东锦湖日丽高分子材料有限公司 | Scratch-resistant polypropylene resin material |
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Application publication date: 20190802 |