CN108059770A - Inorganic filler modifying agent and modified inorganic filler and its preparation method and application and PP composite material and preparation method thereof - Google Patents
Inorganic filler modifying agent and modified inorganic filler and its preparation method and application and PP composite material and preparation method thereof Download PDFInfo
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- CN108059770A CN108059770A CN201610984766.7A CN201610984766A CN108059770A CN 108059770 A CN108059770 A CN 108059770A CN 201610984766 A CN201610984766 A CN 201610984766A CN 108059770 A CN108059770 A CN 108059770A
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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
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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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
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Abstract
The present invention relates to polymeric material fields, specifically provide a kind of inorganic filler modifying agent, which includes：Interfacial compatibilization agent and beta nucleater, wherein, the weight ratio of beta nucleater and Interfacial compatibilization agent is 0.04 2:1.The present invention provides a kind of modified inorganic fillers and its preparation method and application, and this method includes：Inorganic filler, Interfacial compatibilization agent and beta nucleater are uniformly mixed, wherein, inorganic filler is glass fibre and/or talcum.The present invention provides PP composite materials and preparation method thereof.In the present invention, on the basis of traditional rigidity-toughness balanced polypropylene technology, pass through surface nucleation technology and optimization elastomer combination technique, improve the toughness of formula system, rigid particles process for treating surface and Interfacial compatibilization technology, the compatibility of inorganic rigid particle and resin is improved and with reference to power, so as to improve the rigidity of formula system.
Description
Technical field
The present invention relates to a kind of inorganic filler modifying agent and a kind of modified inorganic filler and its preparation method and application and
PP composite material and preparation method thereof.
Background technology
Polypropylene as one of 5 traditional big general-purpose plastics, have price is low, density is small, high temperature resistant, it is resistant to chemical etching,
The shortcomings that the advantages that handling ease, products application is very extensive, but its brittleness is big, and notch impact strength is low also clearly,
Limit the further expansion of its application field.
To improve polyacrylic toughness, it will usually substantial amounts of plasticizer is added in formula system or elastomer is changed
Property, but the addition of either plasticizer or elastomer frequently can lead to the reduction of rigidity, heat resistance, and improve polypropylene
Rigidity adds the inorganic filler of high rigidity mainly in formula system, but due to inorganic filler and polypropylene interface cohesion
Power is relatively low, and the addition of high amount of inorganic filler frequently can lead to the reduction of elongation at break, notch impact strength.
Polypropylene composite of low-temperature flexibility disclosed in CN104592630A and rigidity-toughness balanced and preparation method thereof, by adding
Add the notch impact strength of room temperature and low temperature impact modifying agent raising sample to 66.0KJ/m2, but it bends Young's modulus and exists
Below 100MPa.
CN102311583A discloses a kind of rigidity-toughness balanced polypropylene preparation method, by carrying out group to a variety of acrylic resins
Close, coupling agent treatment carried out to talcum powder, and carried out using toughener it is impact-resistant modified, the rigidity of composition to 2500MPa or so,
But its corresponding impact strength is only 14.1KJ/m2。
CN104592628A improves the rigidity-toughness balanced of system by adding crosslinking agent and assistant crosslinking agent system, composition it is curved
Bent modulus is 1510MPa, notch impact strength 43KJ/m2, and the introducing of cross linker system influences the processing of formula system and breaks
Split the performances such as elongation.
In the prior art, the toughness of system is improved using toughener, the rigidity that inorganic rigid particle improves system is system
Standby high rigidity, the common method of high-toughness polypropylene composition.In published technology, either carried out using toughener tough
Property improve or addition inorganic rigid particle carries out rigid improvement, it is larger due to adding dosage accordingly, it is difficult to simply by
It adjusts proportioning between polypropylene matrix, toughener, inorganic rigid particle three and realizes high rigidity-toughness balanced.
From current published technology, high-rigidity high-ductility polypropene composition bending modulus is substantially in below 2000MPa, greatly
Partly in below 1500MPa, notch impact strength is in 40KJ/m2Hereinafter, it is most of in 30KJ/m2Hereinafter, it is difficult to further simultaneously
Improve the rigidity-toughness balanced of product.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of rigidity that can improve polypropylene material and toughness
Modified inorganic filler.
It, according to the first aspect of the invention, should the present invention provides a kind of inorganic filler modifying agent to realize object defined above
Modifying agent includes：Interfacial compatibilization agent and beta nucleater, wherein, the weight ratio of beta nucleater and Interfacial compatibilization agent is 0.04-2:1.
According to the second aspect of the invention, the present invention provides a kind of preparation method of modified inorganic filler, this method bags
It includes：Inorganic filler, Interfacial compatibilization agent and beta nucleater are uniformly mixed, wherein, inorganic filler is glass fibre and/or talcum.
According to the third aspect of the invention we, the present invention provides the modification nothings that preparation method of the present invention is prepared
Machine filler.
According to the fourth aspect of the invention, the present invention provides modified inorganic filler of the present invention as polymer
Application in additive.
According to the fifth aspect of the invention, the present invention provides a kind of PP composite material, which includes：First group
Divide and the second component；Wherein, the first component includes：(A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E)
Optional coupling agent, (F) optional auxiliary agent；Wherein, the second component includes：(C) modified inorganic filler；The modified inorganic filler
Including modified inorganic filler of the present invention.
According to the sixth aspect of the invention, the present invention provides a kind of preparations of PP composite material of the present invention
Method, wherein, this method includes：First component and the second component are subjected to melting extrusion, drying, granulation, wherein, the first component
Including：(A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E) optional coupling agent, (F) optional auxiliary agent；
Wherein, the second component includes：(C) modified inorganic filler；The modified inorganic filler is filled out including modified inorganic of the present invention
Material.
In the present invention, based on inorganic filler, carried out by using technologies such as interfacial crystallization and Interfacial compatibilizations at surface
Reason, induction filler surface forms fine and close interface scorching and β is brilliant, improves filler and resin boundary surface adhesive strength, so as to significantly carry
The mechanical property of high composite material.
In the present invention, on the basis of traditional rigidity-toughness balanced polypropylene technology, pass through surface nucleation technology and optimization elasticity
Body combination technique improves the toughness of formula system, rigid particles process for treating surface and Interfacial compatibilization technology, improves inorganic rigid
The compatibility of particle and resin and with reference to power, so as to improve the rigidity of formula system.
In a preferred embodiment of the invention, by premixed treatment process and melting extrusion technique, contain in high filler
On the basis of amount, the toughness of PP composite material is improved, PP composite material rigidity is successfully solved and toughness improves simultaneously
Problem, prepare high-rigidity high-ductility PP composite material, further widen the application field of high-rigidity high-ductility polypropene composition.
The PP composite material of the present invention has high-rigidity high-toughness, can meet bending modulus >=2000MPa, notch simultaneously
Impact strength >=50KJ/m2, elongation at break >=200%.And the prior art there is not yet meet bending modulus simultaneously on a kind of
>=2000MPa, notch impact strength >=50KJ/m2, the high-rigidity high-ductility PP composite material of elongation at break >=200% and its
The report of preparation method.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The endpoint of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For numberical range, between the endpoint value of each scope, respectively
It between the endpoint value of a scope and individual point value and can be individually combined with each other between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
In the present invention, as without opposite explanation, then percentage refers to weight percent, and number refers to parts by weight.In addition, such as
Without illustrating, all operations carry out at normal temperatures and pressures.
The present invention provides a kind of inorganic filler modifying agent, which includes：Interfacial compatibilization agent and beta nucleater, wherein,
Beta nucleater and the weight ratio of Interfacial compatibilization agent are 0.04-2:1.
, according to the invention it is preferred to the beta nucleater and the weight ratio of Interfacial compatibilization agent are 0.2-0.5:1.
According to the present invention, the beta nucleater refers to that out-phase nucleation can be played during polyolefin crystallization
Substance its object is to change the crystallization behavior of resin, has effects that improve crystalline rate, crystallinity and beta crystal conversion ratio
A kind of substance, optional wider range of species, common beta nucleater may be incorporated for the present invention, for the present invention, preferably
The beta nucleater is selected from the one of rare earth organic complex, organic phosphate nucleating agent, dibenzal sorbitol and fragrant amide compound
Kind is a variety of, more preferably rare earth organic complex.
In the present invention, the rare earth organic complex, organic phosphate nucleating agent, dibenzal sorbitol and fragrant amide compound
The species of object selects optional wider range, can be conventional selection, such as the rare earth organic complex is organic condensed hetero ring ring
Compound, fused ring compound, aliphatic carboxylic acid and its derivative, aromatic carboxylic acid and its derivative or other kinds of ligand with
The lanthanide series of rare earth element, wherein the one or more in the complex formed with rare earth elements such as lanthanum, cerium, praseodymium, neodymium, yttriums.
In the present invention, preferably described organic phosphate nucleating agent for phosphate metal salt and phosphate basic metal salt and its
One or more in compound.
In the present invention, preferably described fragrant amide compound is 2,6- cyclohexanedimethanols amide and/or terephthalic acid (TPA) ring
One or more in hexane amide.
In an embodiment of the present invention, using rare earth organic complex WBG-II, (the bright woods in Guangdong receives functional material to beta nucleater
Co., Ltd) it is used as exemplary illustration.
In the present invention, the Interfacial compatibilization agent refers to compatibility between increase polymer blend components, and strengthens polymerization
A kind of polymer or small molecule systems of bonding interface between object, it is scattered in resin system its object is to improve filler
Degree, the interface compatibility of raising filler and PP resins, optional wider range, for the present invention, preferably described Interfacial compatibilization agent
It is preferably polar monomer graft polymer and silane coupling agent selected from polar monomer graft polymer and/or silane coupling agent
The weight ratio of mixture, more preferable silane coupling agent and polar monomer graft polymer is 0.1-10:1, more preferably 0.3-4:
1。
In the present invention, optional wider range of the polar monomer, for the present invention, preferably described polar monomer is selected from acid
One kind or more in acid anhydride, carboxylic acid and its derivative, amine compound, hydroxy compounds, epoxide and ionic compound
Kind.
According to the present invention, acid anhydrides is, for example, the one or more in methacrylic anhydride, maleic anhydride and itaconic anhydride.
According to the present invention, carboxylic acid and its derivative are, for example, acrylic acid, methacrylic acid, itaconic acid, maleic acid and Fu Ma
One or more in acid.
According to the present invention, amine compound is containing the one or more in primary amine and secondary amine compound.
According to the present invention, hydroxy compounds is for one in (methyl) hydroxy-ethyl acrylate and (methyl) hydroxypropyl acrylate
Kind is a variety of.
According to the present invention, epoxides is the one or more in phenylglycidyl ether and ethylene oxide.
According to the present invention, ionic compound is the one or more in sulfonate, carboxylate, phosphate and quaternary amine.
According to the present invention, the silane coupling agent is one kind or more in amino silicane coupling agent and epoxy silane coupling agent
Kind.
According to the present invention, the polar monomer graft polymer is maleic anhydride inoculated polypropylene.
A preferred embodiment of the invention, the bulking agent are grafted poly- third for silane coupling agent and maleic anhydride
The mixture of alkene (MAH-PP).
According to the present invention, the grafting rate of the maleic anhydride inoculated polypropylene is 1-5%.
The purpose of the achievable benzene invention of aforementioned modifiers modified inorganic filler using the present invention, according to the present invention one
Kind preferred embodiment, the present invention provides a kind of preparation method of modified inorganic filler, this method includes：By inorganic filler,
Interfacial compatibilization agent, beta nucleater are uniformly mixed, wherein, inorganic filler is glass fibre and/or talcum.
With the method for the invention it is preferred to beta nucleater and the weight ratio of Interfacial compatibilization agent are 0.04-2:1, it is preferably 0.2-
0.5:1。
The species of the method according to the invention, the beta nucleater and Interfacial compatibilization agent has been discussed in detail foregoing, herein
It repeats no more.
With the method for the invention it is preferred to which the inorganic filler is talcum powder, more preferable talcum powder is the cunning of high length-diameter ratio
Mountain flour, preferably draw ratio >=15 of more preferable talcum powder, draw ratio >=30, mesh number are 2000-8000 mesh, are preferably 3000-
5000 mesh.
With the method for the invention it is preferred to the step of mixing, includes：The first mixing and the second mixing are successively carried out, the
The rotating speed of two mixing is higher than the rotating speed of the first mixing.
A preferred embodiment of the invention, the rotating speed of the first mixing is 10-100rpm, the rotating speed of the second mixing
For 100-1000rpm.
The time of a preferred embodiment of the invention, the time of the first mixing and the second mixing is respectively 3-
5min。
The temperature of a preferred embodiment of the invention, the temperature of the first mixing and the second mixing is respectively 60-
120℃。
With the method for the invention it is preferred to compared with 100 parts of inorganic filler dosage, the Interfacial compatibilization agent is nucleated with β
Total dosage of agent is 3-15 parts, is preferably 6-10 parts.
The present invention provides the modified inorganic fillers being prepared according to preparation method of the present invention.
The present invention provides modified inorganic filler of the present invention as the application in polymeric additive.
The present invention provides a kind of PP composite material, which includes：First component and the second component；
Wherein, the first component includes：(A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E) are optional
Coupling agent, (F) optional auxiliary agent；
Wherein, the second component includes：(C) modified inorganic filler；The modified inorganic filler includes of the present invention change
Property inorganic filler.
According to the present invention, the PP composite material has excellent rigidity, strong according to the test bendings of standard ISO 178
Degree, bending modulus >=2000MPa；With excellent toughness, notch impact strength, notch are tested according to standard ISO 179/1eA
Impact strength >=50KJ/m2；With excellent non-deformability, elongation at break is tested according to standard ISO 527-2, fracture is stretched
Long rate >=200%.
A preferred embodiment of the invention, by weight, the material include：First 60-80 parts of component, second
20-60 parts of component.
A preferred embodiment of the invention, wherein, the first component includes by weight：(A) polypropylene 40-70
Part, it is preferably 45-60 parts；(B) polyolefin elastomer 5-20 parts, be preferably 10-15 parts；(D) optional 0.5-6 parts of bulking agent,
Preferably 1-5 parts；(E) optional 0.3-3 parts of coupling agent is preferably 0.5-1.5 parts；(F) optional auxiliary agent：0.2-5 parts, preferably
For 0.3-1.5 parts.
A kind of more preferable embodiment according to the present invention, on the basis of weight, 2≤component (A)/component (B)≤14, more
It is preferred that 3≤component (A)/component (B)≤6.
According to the present invention, to component (A) polypropylene without particular/special requirement, for the present invention, preferred ingredient (A) is polyacrylic molten
Body flow rate≤5g/10min, preferably≤3g/10min.
, according to the invention it is preferred to component (A) polypropylene gathers selected from homopolypropylene, block copolymerization polypropylene and random copolymerization
The one or more of propylene.It is, for example, specifically homopolypropylene L5E89, atactic copolymerized polypropene C4220 and block copolymerization poly- third
One or more in alkene BA212E.
According to the present invention, for the species of component (B) polyolefin elastomer without particular/special requirement, it is one to refer to polyolefin
Kind High performance polyolefin product, is presented caoutchouc elasticity at normal temperatures, with density is small, bending is big, low-temperature impact resistance is high, easy
The features such as processing, for the present invention, the one or more being preferably selected from based elastomers and propylene-based elastomeric, vinyl
Elastomer is, for example, ethylene-octene copolymer.Specific is, for example, the one or more in POE, OBC and PBE.
According to the present invention, component (D) bulking agent is preferably maleic anhydride inoculated polypropylene, for the present invention, preferably Malaysia
Anhydride-grafted polypropylene melt flow rate (MFR) is 10-400g/10min, more preferably 50-200g/10min, more preferable maleic acid
The grafting rate of acid anhydride is 0.8-2%, is preferably 1-1.5%.
, according to the invention it is preferred to which maleic anhydride inoculated polypropylene shape is powder, mesh number is 10-200 mesh, more preferably
30-100 mesh.
According to the present invention, without particular/special requirement, coupling agent commonly used in the art may be incorporated for the species of component (E) coupling agent
The present invention, for the present invention, the one or more being preferably selected from titanate coupling agent and silane coupling agent, more preferably silicon
Alkane coupling agent.
According to the present invention, for the species of component (F) auxiliary agent without particular/special requirement, auxiliary agent commonly used in the art is used equally for this hair
It is bright, for the present invention, the one or more in lubricant, antioxidant, light stabilizer, nucleating agent and pigment are preferably included, are lubricated
Agent is preferably calcium stearate.
In the present invention, antioxidant is, for example, primary antioxidant and auxiliary antioxidant according to 1:The B225 that 1 compounding obtains, dosage
For example, 0.2-1.5 parts, preferred dosage is 0.3-0.5 parts.
The present invention provides a kind of preparation method of the foregoing PP composite material of present invention, wherein, this method includes：
First component and the second component are subjected to melting extrusion, drying, granulation, wherein, the first component includes：(A) polypropylene, (B) are poly-
Olefin elastomer, (D) optional bulking agent, (E) optional coupling agent, (F) optional auxiliary agent；Wherein, the second component includes：
(C) modified inorganic filler；The modified inorganic filler includes modified inorganic filler of the present invention.
A preferred embodiment of the invention, the condition of melting extrusion include：Temperature is 180-280 DEG C, rotating speed
For 50-500rpm, residence time of material 1-10min.
A preferred embodiment of the invention, the preparation method of PP composite material include：
(1) by (A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E) optional coupling agent and (F) can
Auxiliary agent of choosing etc. is put into high-speed mixer for dry mixing 3-5min, and the main feeding bin for being positioned over double screw extruder after mixing is standby
With；(C) modified inorganic filler is added in the side spout of double screw extruder；
(2) main feeding bin material and side spout material are subjected to melting extrusion by double screw extruder, air-dry, make
Grain, obtains meeting material.
A preferred embodiment of the invention, 150-240 DEG C of host temperature, engine speed in 150-450rpm,
Residence time of the material in machine barrel about 0.5-3min, so as to ensure blending and plasticizing effect well.
The PP composite material of the present invention has excellent rigidity, and bending strength is tested according to standard ISO 178, curved
Bent modulus >=2000MPa；With excellent toughness, notch impact strength is tested according to standard ISO 179/1eA, notch shock is strong
Degree >=50KJ/m2；With excellent non-deformability, elongation at break is tested according to standard ISO 527-2, elongation at break >=
200%.
The preparation method of PP composite material provided by the invention, on the basis of traditional rigidity-toughness balanced polypropylene technology
On, by surface nucleation technology and optimize elastomer combination technique, improve the toughness of formula system, rigid particles surface treatment skill
Art and Interfacial compatibilization technology improve the compatibility of inorganic rigid particle and resin and with reference to power, so as to improve the firm of formula system
Property.The present invention on the basis of high filler content, improves polypropylene composite materials by premixed treatment process and melting extrusion technique
The toughness of material successfully solves the problems, such as PP composite material rigidity and toughness while improves, prepares high-rigidity high-ductility poly- third
Alkene composite material has further widened the application field of high-rigidity high-ductility PP composite material.
Embodiment 1
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies), 1.5 parts of MAH-PP powder (100 mesh,
Grafting rate 1.0%), 1.2 parts of beta nucleaters (WBG-II, Guangdong Weilinna Function Materials Co., Ltd) and 1.5 parts it is silane coupled
Being positioned over the high-speed mixer with heating function, (temperature setting is 80 for agent (KH-570, Chengdu development Chemical Co., Ltd.)
DEG C) in low speed (rotating speed 50rpm, remaining embodiment are identical with comparative example) mixing 3min, at a high speed (rotating speed 200rpm, remaining
Embodiment is identical with comparative example) mixing 5min, (C) modified talc powder is obtained after mixing and 9 parts of transferase 12 is to twin-screw extrusion
The side spout of machine；
By 26 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 30 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 14 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C) and 1 part of auxiliary agent (0.5 part of calcium stearate, Shijiazhuang Yongfeng chemical plastic auxiliary reagent factory,
0.5 part of antioxidant B225, BASF AG) high-speed mixer for dry mixing 3min is put into, 71 parts are shifted after mixing to twin-screw
The main spout of extruder；
(processing temperature 150- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
240 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2025MPa, notch impact strength
=69.4KJ/m2, elongation at break=297%.
Embodiment 2
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies), 1.8 parts of MAH-PP powder (100 mesh,
Grafting rate 1.0%), 0.6 part of beta nucleater (WBG-II, Guangdong Weilinna Function Materials Co., Ltd) and 1.8 parts it is silane coupled
Being positioned over the high-speed mixer with heating function, (temperature setting is 90 for agent (KH-570, Chengdu development Chemical Co., Ltd.)
DEG C) in mixed on low speed 3min, mixed at high speed 5min, obtain (C) modified talc powder after mixing and shift 34 parts to twin-screw
The side spout of extruder；
By 15 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 15 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 20 parts of propylene-based block copolymer (PPB,
BA212E, MI=0.3g/10min, 2.16kg, 230 DEG C), 15 parts of ethylene-octene copolymers (POE, 8150, MI=0.5g/
10min, 2.16kg, 190 DEG C) and 1 part of auxiliary agent (0.7 part of lubricant stearic acid calcium, Shijiazhuang Yongfeng chemical plastic auxiliary reagent factory, 0.3
Part antioxidant B225, BASF AG) high-speed mixer for dry mixing 3min is put into, 66 parts are shifted after mixing to twin-screw extrusion
The main spout of machine；
After above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder (processing temperature for 150~
240 DEG C, engine speed is in 200rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of polypropylene composite materials of high rigidity-toughness balanced
Material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2078MPa, notch impact strength
=64.9KJ/m2, elongation at break=274%.
Embodiment 3
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies), 1.5 parts of MAH-PP powder (100 mesh,
Grafting rate 1.0%), 1.2 parts of beta nucleaters (WBG-II, Guangdong Weilinna Function Materials Co., Ltd) and 1.5 parts it is silane coupled
Being positioned over the high-speed mixer with heating function, (temperature setting is 80 for agent (KH-570, Chengdu development Chemical Co., Ltd.)
DEG C) in mixed on low speed 3min, mixed at high speed 5min, obtain (C) modified talc powder after mixing and 9 parts of transferase 12 be to twin-screw
The side spout of extruder；
By 24 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 36 parts of propylene
Block copolymer (PPB, BA212E, MI=0.3g/10min, 2.16kg, 230 DEG C), 6 parts of ethylene-octene copolymers (POE,
8150, MI=0.5g/10min, 2.16kg, 190 DEG C) and 4 parts of propylene-based elastomerics (PBE, 6102, MI=3.0g/10min,
2.16kg, 230 DEG C), 1 part of auxiliary agent (0.5 part of lubricant stearic acid calcium, Shijiazhuang Yongfeng chemical plastic auxiliary reagent factory, 0.5 part of antioxygen
Agent B225, BASF AG) high-speed mixer for dry mixing 3min is put into, 71 parts of masters to double screw extruder are shifted after mixing
Spout；
(processing temperature 150- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
230 DEG C, engine speed is in 350rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of Polypropylene compositions of high rigidity-toughness balanced
Object.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2537MPa, notch impact strength
=53.4KJ/m2, elongation at break=211%.
Embodiment 4
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies), 1.8 parts of MAH-PP powder (100 mesh,
Grafting rate 1.0%), 0.6 part of beta nucleater (WBG-II, Guangdong Weilinna Function Materials Co., Ltd) and 1.8 parts it is silane coupled
Being positioned over the high-speed mixer with heating function, (temperature setting is 90 for agent (KH-570, Chengdu development Chemical Co., Ltd.)
DEG C) in mixed on low speed 3min, mixed at high speed 5min, obtain (C) post processing talcum powder after mixing and shift 34 parts to double spiral shells
The side spout of bar extruder；
By 17.5 parts of homopolypropylene (PPH, T30S, MI=3.0g/10min, 2.16kg, 230 DEG C), 17.5 parts of propylene
Random copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 15 parts of propylene-based block copolymer (PPB,
H2483, MI=0.3g/10min, 2.16kg, 230 DEG C), 15 parts of ethylene-octene copolymers (POE, 8150, MI=0.5g/
10min, 2.16kg, 190 DEG C), and 1 part of auxiliary agent (0.7 part of lubricant stearic acid calcium, Shijiazhuang Yongfeng chemical plastic auxiliary reagent factory, 0.3
Part antioxidant B225, BASF AG) high-speed mixer for dry mixing 3min is put into, 66 parts are shifted after mixing to twin-screw extrusion
The main spout of machine；
(processing temperature 160- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
230 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of polypropylene composite materials of high rigidity-toughness balanced
Material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2200MPa, notch impact strength
=55.9KJ/m2, elongation at break=233%.
1 each embodiment composition of raw materials of table and the performance test results
Comparative example 1
By 29 parts of talcum powder (trades mark3CA, French IMERYS companies) be positioned over double screw extruder side feed
Material mouth；
30 parts of homopolypropylene (PPH, T30S, MI=3.0g/10min, 2.16kg, 230 DEG C), 36 parts of propylene is embedding
Section copolymer (PPB, BA212E, MI=0.3g/10min, 2.16kg, 230 DEG C), 4 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C), (0.5 part of lubricant stearic acid calcium, Shijiazhuang Yongfeng chemical plastic help 1 part of auxiliary agent
Agent factory, 0.5 part of antioxidant B225, BASF AG) high-speed mixer for dry mixing 3min is put into, 71 parts are shifted after mixing to double
The main spout of screw rod；
After above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder (processing temperature for 160~
220 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2716MPa, notch impact strength
=20.6KJ/m2, elongation at break=116%.
Comparative example 2
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies) and 1.5 parts of silane coupling agent (KH-
570, Chengdu development Chemical Co., Ltd.) be positioned over it is low in the high-speed mixer with heating function (temperature setting is at 80 DEG C)
Speed mixes 3min, mixed at high speed 5min, after mixing 9 parts of side spouts to double screw extruder of transferase 12；
By 26 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 30 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 14 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C), 1 part of other auxiliary agents (0.5 part of lubricant stearic acid calcium, the modeling of Shijiazhuang Yongfeng chemical industry
Expect auxiliary reagent factory, 0.5 part of antioxidant B225, BASF AG) etc. be put into high-speed mixer for dry mixing 3min, shift 71 after mixing
Part to the main spout of twin-screw；
(processing temperature 160- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
220 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=1990MPa, notch impact strength
=48.7KJ/m2, elongation at break=319%.
Comparative example 3
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies) and 1.5 parts of MAH-PP powder (100 mesh,
Grafting rate 1.0%) mixed on low speed 3min in the high-speed mixer with heating function (temperature setting is at 80 DEG C) is positioned over, at a high speed
5min is mixed, after mixing 9 parts of side spouts to double screw extruder of transferase 12；
By 26 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 30 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 14 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C), 1 part of other auxiliary agents (0.5 part of lubricant stearic acid calcium, the modeling of Shijiazhuang Yongfeng chemical industry
Expect auxiliary reagent factory, 0.5 part of antioxidant B225, BASF AG) etc. be put into high-speed mixer for dry mixing 3min, shift 71 after mixing
Part to the main spout of twin-screw；
(processing temperature 160- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
220 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=2069MPa, notch impact strength
=44.1KJ/m2, elongation at break=208%.
Comparative example 4
By 100 parts of talcum powder (trades mark3CA, French IMERYS companies) and 1.2 parts of beta nucleaters (WBG-II, extensively
Dong Weilinna functional materials Co., Ltd), it is positioned over low in the high-speed mixer with heating function (temperature setting is at 80 DEG C)
Speed mixes 3min, mixed at high speed 5min, after mixing 9 parts of side spouts to double screw extruder of transferase 12；
By 26 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 30 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 14 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C), 1 part of other auxiliary agents (0.5 part of lubricant stearic acid calcium, the modeling of Shijiazhuang Yongfeng chemical industry
Expect auxiliary reagent factory, 0.5 part of antioxidant B225, BASF AG) etc. be put into high-speed mixer for dry mixing 3min, shift 71 after mixing
Part to the main spout of twin-screw；
(processing temperature 160- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
220 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=1860MPa, notch impact strength
=63.3KJ/m2, elongation at break=432%.
Comparative example 5
By 29 parts of talcum powder (trades mark3CA, French IMERYS companies) be positioned over double screw extruder side feed
Material mouth；
By 26 parts of homopolypropylene (PPH, L5E89, MI=3.0g/10min, 2.16kg, 230 DEG C), 30 parts of propylene without
Advise copolymer (PPR, C4220, MI=0.5g/10min, 2.16kg, 230 DEG C), 14 parts of ethylene-octene copolymers (POE, 8150,
MI=0.5g/10min, 2.16kg, 190 DEG C), 0.5 part of MAH-PP powder (100 mesh, grafting rate 1.0%), 0.4 part of beta nucleater
(WBG-II, Guangdong Weilinna Function Materials Co., Ltd), (KH-570, Chengdu development chemical industry are limited for 0.5 part of silane coupling agent
Company), 1 part of other auxiliary agents (0.5 part of lubricant stearic acid calcium, Shijiazhuang Yongfeng chemical plastic auxiliary reagent factory, 0.5 part of antioxidant
B225, BASF AG) etc. be put into high-speed mixer for dry mixing 3min, shift 71 parts after mixing to the main spout of twin-screw；
(processing temperature 160- after above-mentioned material is added in by the main feeding and side feeding measurement of double screw extruder
220 DEG C, engine speed is in 300rpm) melting extrusion is carried out, air-dries, be granulated, obtain a kind of high-rigidity high-ductility PP composite material.
The performance test results of the high-rigidity high-ductility PP composite material：Bending modulus=1967MPa, notch impact strength
=52.1KJ/m2, elongation at break=287%.
2 each comparative example composition of raw materials of table and the performance test results
By carrying out premixed treatment process and melting extrusion work to talcum powder it can be seen from the result of Tables 1 and 2
Skill on the basis of high filler content, improves the toughness of PP composite material, successfully solve PP composite material rigidity and
The problem that toughness improves simultaneously prepares high-rigidity high-ductility PP composite material and meets bending modulus >=2000MPa, notch punching simultaneously
Hit intensity >=50KJ/m2, elongation at break >=200%.Further widen the application field of high-rigidity high-ductility polypropene composition.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that the specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (13)
1. a kind of inorganic filler modifying agent, which is characterized in that the modifying agent includes：Interfacial compatibilization agent and beta nucleater, wherein, β into
The weight ratio of core agent and Interfacial compatibilization agent is 0.04-2:1.
2. modifying agent according to claim 1, wherein,
The beta nucleater and the weight ratio of Interfacial compatibilization agent are 0.2-0.5:1；
The beta nucleater is selected from rare earth organic complex, organic phosphate nucleating agent, dibenzal sorbitol and fragrant amide compound
One or more, be preferably rare earth organic complex；
The Interfacial compatibilization agent is selected from polar monomer graft polymer and/or silane coupling agent, is preferably that polar monomer graft gathers
The weight ratio of the mixture of conjunction object and silane coupling agent, more preferable silane coupling agent and polar monomer graft polymer is 0.1-
10:1, more preferably 0.3-4:1；
It is preferred that the polar monomer is selected from acid anhydrides, carboxylic acid, carboxylic acid derivates, amine compound, hydroxy compounds, epoxide
With the one or more in ionic compound, the silane coupling agent is in amino silicane coupling agent and epoxy silane coupling agent
One or more.
3. a kind of preparation method of modified inorganic filler, this method include：Inorganic filler, Interfacial compatibilization agent, beta nucleater are mixed
Uniformly, wherein, inorganic filler is glass fibre and/or talcum.
4. preparation method according to claim 3, wherein,
Beta nucleater and the weight ratio of Interfacial compatibilization agent are 0.04-2:1, it is preferably 0.2-0.5:1；
The beta nucleater is selected from rare earth organic complex, organic phosphate nucleating agent, dibenzal sorbitol and fragrant amide compound
One or more, be preferably rare earth organic complex；
The Interfacial compatibilization agent is selected from polar monomer graft polymer and/or silane coupling agent, is preferably that polar monomer graft gathers
The weight ratio of the mixture of conjunction object and silane coupling agent, more preferable silane coupling agent and polar monomer graft polymer is 0.1-
10:1, more preferably 0.3-4:1；
It is preferred that the polar monomer is selected from acid anhydrides, carboxylic acid, carboxylic acid derivates, amine compound, hydroxy compounds, epoxide
With the one or more in ionic compound；
The silane coupling agent is the one or more in amino silicane coupling agent and epoxy silane coupling agent；
The inorganic filler be talcum powder, draw ratio >=15 of preferably talc powder, preferably draw ratio >=30, mesh number 2000-
8000 mesh are preferably 3000-5000 mesh.
5. the preparation method according to claim 3 or 4, wherein,
The step of mixing, includes：The first mixing and the second mixing are successively carried out, the rotating speed of the second mixing is higher than the first mixing
Rotating speed；
It is preferred that the rotating speed of the first mixing is 10-100rpm, the rotating speed of the second mixing is 100-1000rpm；
The time of more preferable first mixing and the time of the second mixing are respectively 3-5min；
The temperature of further preferred first mixing and the temperature of the second mixing are respectively 60-120 DEG C.
6. the preparation method according to claim 3 or 4, wherein, compared with 100 parts of inorganic filler dosage, the interface
Total dosage of bulking agent and beta nucleater is 3-15 parts, is preferably 6-10 parts.
7. the modified inorganic filler that the preparation method in claim 3-6 described in any one is prepared.
8. the modified inorganic filler described in claim 7 is as the application in polymeric additive.
9. a kind of PP composite material, which is characterized in that the material includes：First component and the second component；
Wherein, the first component includes：(A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E) are optionally coupled
Agent, (F) optional auxiliary agent；
Wherein, the second component includes：(C) modified inorganic filler；
Wherein, the modified inorganic filler includes the modified inorganic filler described in claim 7.
10. composite material according to claim 9, wherein, by weight, which includes：
First 60-80 parts of component, the second 20-60 parts of component；
Wherein, the first component includes by weight：(A) polypropylene 40-70 parts, be preferably 45-60 parts；(B) polyolefin elastomer
5-20 parts, be preferably 10-15 parts；(D) optional 0.5-6 parts of bulking agent is preferably 1-5 parts；(E) optional coupling agent 0.3-3
Part, it is preferably 0.5-1.5 parts；(F) optional auxiliary agent：0.2-5 parts, be preferably 0.3-1.5 parts；
It is preferred that on the basis of weight, 2≤component (A)/component (B)≤14, more preferable 3≤component (A)/component (B)≤6.
11. the composite material according to claim 9 or 10, wherein,
Component (A) polyacrylic melt flow rate (MFR)≤5g/10min, preferably≤3g/10min；
Preferred ingredient (A) polypropylene is selected from homopolypropylene, one kind or more of block copolymerization polypropylene and atactic copolymerized polypropene
Kind；
One or more of component (B) polyolefin elastomer in based elastomers and propylene-based elastomeric；
Component (D) bulking agent is maleic anhydride inoculated polypropylene, and the melt flow rate (MFR) of preferably maleic anhydride inoculated polypropylene is
10-400g/10min is preferably 50-200g/10min, and the grafting rate of maleic anhydride is 0.8-2%, is preferably 1-1.5%；
It is preferred that maleic anhydride inoculated polypropylene shape is powder, mesh number is 10-200 mesh, is preferably 30-100 mesh；
Component (E) coupling agent is the one or more in titanate coupling agent and silane coupling agent, preferably silane coupled
Agent；
Component (F) auxiliary agent includes the one or more in lubricant, antioxidant, light stabilizer, nucleating agent and pigment, and lubricant is excellent
Elect calcium stearate as.
12. a kind of preparation method of the PP composite material in claim 9-11 described in any one, wherein, this method bag
It includes：First component and the second component are subjected to melting extrusion, drying, granulation,
Wherein, the first component includes：(A) polypropylene, (B) polyolefin elastomer, (D) optional bulking agent, (E) are optionally coupled
Agent, (F) optional auxiliary agent；
Wherein, the second component includes：(C) modified inorganic filler；
The modified inorganic filler includes the modified inorganic filler described in claim 7.
13. preparation method according to claim 12, wherein, the condition of melting extrusion includes：Temperature is 180-280 DEG C,
Rotating speed is 50-500rpm, residence time of material 1-10min.
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| CN110218394A (en) * | 2019-05-24 | 2019-09-10 | 骆驼集团塑胶制品有限公司 | A kind of electrolyte resistance polypropylene modified material of low temperature ultra-toughness and preparation method thereof |
| CN110951156A (en) * | 2018-09-26 | 2020-04-03 | 合肥杰事杰新材料股份有限公司 | Polypropylene composite material with high surface tension and excellent comprehensive performance and preparation method thereof |
| CN112538215A (en) * | 2019-09-20 | 2021-03-23 | 茂名骐锋新材料有限公司 | Impact-resistant low-temperature-resistant high-transparency polypropylene composition |
| CN112552594A (en) * | 2020-12-09 | 2021-03-26 | 重庆澳彩新材料股份有限公司 | Polypropylene-based composite material, preparation method thereof and high-tensile MPP pipeline |
| CN114410013A (en) * | 2022-01-17 | 2022-04-29 | 上海金发科技发展有限公司 | Talcum powder filled polypropylene composite material and preparation method and application thereof |
| CN114507399A (en) * | 2022-03-24 | 2022-05-17 | 成都金发科技新材料有限公司 | Polypropylene material and preparation method and application thereof |
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| CN112552594A (en) * | 2020-12-09 | 2021-03-26 | 重庆澳彩新材料股份有限公司 | Polypropylene-based composite material, preparation method thereof and high-tensile MPP pipeline |
| CN114410013A (en) * | 2022-01-17 | 2022-04-29 | 上海金发科技发展有限公司 | Talcum powder filled polypropylene composite material and preparation method and application thereof |
| CN114507399A (en) * | 2022-03-24 | 2022-05-17 | 成都金发科技新材料有限公司 | Polypropylene material and preparation method and application thereof |
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