CN102952336A - Active basic magnesium sulfate whisker modified polypropylene composite material and preparation method thereof - Google Patents
Active basic magnesium sulfate whisker modified polypropylene composite material and preparation method thereof Download PDFInfo
- Publication number
- CN102952336A CN102952336A CN2012104581599A CN201210458159A CN102952336A CN 102952336 A CN102952336 A CN 102952336A CN 2012104581599 A CN2012104581599 A CN 2012104581599A CN 201210458159 A CN201210458159 A CN 201210458159A CN 102952336 A CN102952336 A CN 102952336A
- Authority
- CN
- China
- Prior art keywords
- magnesium sulfate
- crystal whisker
- sulfate crystal
- composite material
- alkali magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 130
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 65
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 65
- -1 polypropylene Polymers 0.000 title claims abstract description 59
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 55
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000012895 dilution Substances 0.000 claims abstract description 12
- 238000010790 dilution Methods 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 66
- 239000003513 alkali Substances 0.000 claims description 62
- 239000003381 stabilizer Substances 0.000 claims description 25
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 150000002148 esters Chemical class 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 11
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000005453 pelletization Methods 0.000 claims description 9
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- WNFDFOPVGKYQOF-UHFFFAOYSA-N C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)P(O)(O)O Chemical class C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)P(O)(O)O WNFDFOPVGKYQOF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 150000003568 thioethers Chemical class 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 150000005002 naphthylamines Chemical class 0.000 claims description 3
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000012760 heat stabilizer Substances 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000004033 plastic Substances 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 8
- 239000006087 Silane Coupling Agent Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 229920005629 polypropylene homopolymer Polymers 0.000 description 6
- 230000035939 shock Effects 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- 241001131796 Botaurus stellaris Species 0.000 description 2
- 101100522110 Oryza sativa subsp. japonica PHT1-10 gene Proteins 0.000 description 2
- 101100522109 Pinus taeda PT10 gene Proteins 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000013535 sea water Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001897 terpolymer Polymers 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- LAZOHFXCELVBBV-UHFFFAOYSA-N [Mg].[Ca].[Si] Chemical compound [Mg].[Ca].[Si] LAZOHFXCELVBBV-UHFFFAOYSA-N 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Classifications
-
- 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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- 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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- 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
-
- 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
-
- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an active basic magnesium sulfate whisker modified polypropylene composite material and a preparation method thereof. The composite material consists of polypropylene, basic magnesium sulfate whiskers, a flexibilizer, a processing agent, a coupling agent, acid dilution and a heat stabilizer. An engineering part made of the composite material disclosed by the invention is developed towards the lightweight; the composite material is beneficial to the reduction of the use quantity of the material and the reduction of the use cost of the material; and moreover, the product is green and environmental-friendly and is suitable to prepare automobile interior parts.
Description
Technical field
The invention belongs to technical field of polymer composite materials, be specifically related to a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material and preparation method thereof.
Technical background
Polypropylene is a kind of general plastics, but the inner and outer decorative parts at fabrication parts such as automobile, because its intensity, rigidity and resistance toheat can not satisfy the requirement of parts, polyacrylic impact property is poor simultaneously, particularly low-temperature impact is poor, and its molding shrinkage is large, these drawbacks limit application and the development of polypropylene in engineering part.So the material for preparing at present inner and outer decorative parts of automobile mainly is to make by adding conventional breeze filled modified polypropylene, its product has good, the easy machine-shaping of size, the advantage such as cheap.But along with the lightweight cry of automobile in recent years is more and more higher, over-all properties is high, low density modified plastics more and more comes into one's own.Wherein whisker is exactly a kind of good combination property, can replaces conventional breeze even fiber to satisfy the requirement of inner and outer decorative parts of automobile material.
Whisker refers to a kind of staple fibre of growing into high purity monocrystalline form under the manual control condition, its diameter very little (micron number magnitude), do not contain the defective (crystal boundary, dislocation, hole etc.) that exists in the common material, its atomic arrangement high-sequential, thereby its intensity is close to the theoretical value of perfect crystal.Its height-oriented structure not only makes it have high strength, high-modulus and high elongation rate, but also has electricity, light, magnetic, dielectric, conduction, superconduction character.The intensity of whisker mainly is used as the enhancing body of matrix material, for the manufacture of high strength composite far above other chopped strands.The kind of whisker is a lot, such as silicon carbide whisker, aluminium borate whisker, potassium titanate crystal whisker, calcium carbonate crystal whisker, alkali magnesium sulfate crystal whisker, ZnOw, calcium sulfate crystal whiskers and silicon-calcium-magnesium whisker etc.
Relatively comprehensive, the performance of alkali magnesium sulfate crystal whisker is best in all whiskers, be mainly manifested in the characteristics such as the intensity modulus is high, density is low, can be used as the strengthening and toughening agent of the matrix materials such as plastics, rubber and resin, improve flexural strength and the resistance to impact shock of body material.In addition, its coefficient of expansion and plastics are close, and are good with the consistency of plastics.Also have nontoxic, thermal value is little, the characteristic such as fire-retardant.After alkali magnesium sulfate crystal whisker and plastics, rubber are made matrix material, not only have good strengthening and toughening effect, and outward appearance is good, excellent rigidity, shock resistance is strong, and volumetric shrinkage is extremely low, dimensional precision is high, and the heat resistanceheat resistant performance is good, also can give the flame retardant properties of matrix material.
Summary of the invention
The present invention is directed to problems of the prior art, a kind of high strength, high-modulus, low density, low-shrinkage, machine-shaping property is good and comprehensive mechanical property is good active alkali magnesium sulfate crystal whisker modified polypropylene composite material are provided.Another object of the present invention provides the preparation method of above-mentioned active alkali magnesium sulfate crystal whisker modified polypropylene composite material.
In order to achieve the above object, the present invention realizes by following technical proposal:
A kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material, the weight part of its constitutive material is:
Polypropylene: 50-88 part;
Alkali magnesium sulfate crystal whisker: 10-40 part;
Toughner: 2-10 part;
Processing aid: 0.1-1 part;
Coupling agent: 0.3-0.5 part;
Acid dilution: 0.3-0.5;
Thermo-stabilizer: 0.1-1 part.
Described polypropylene is at least a in homopolymerization polypropylene, the Co-polypropylene, and its melting index is 10-25g/10min.
The length-to-diameter ratio of described alkali magnesium sulfate crystal whisker is that 10-30, particle diameter are 0.5-4um.
Described toughner is vinyl elastomerics or styrenic elastomerics, and the present invention preferentially selects polyethylene (PE), ethylene-octene polymkeric substance (POE), ethylene-propylene-butadiene terpolymer (EPDM).
Described processing aid is calcium stearate (Ca-St
2), at least a in the ethylene bis stearamide (EBS), modification ethylene bis stearamide (TAF).
Described coupling agent is a kind of for being selected among silicane KH550, KH560, the KH570, or a kind of among titanate ester NDZ-101, the NDZ-40.
Described sour dilution is at least a aqueous solution that forms with the water configuration in hydrochloric acid, sulfuric acid, the phosphoric acid, and the volume percent of described sour dilution is 0.5-2%.
Described thermo-stabilizer is selected from 2, three grades of butyl of 6--4-methylphenol, two (3, three grades of butyl of 5--4-hydroxy phenyl) thioether, four (β-(3, three grades of butyl of 5--4-hydroxy phenyl) propionic acid) at least a in three (2,4-di-tert-butyl-phenyl) phosphorous acid esters (168) of pentaerythritol ester (1010), phosphorous acid lipid, three monooctyl esters, three last of the ten Heavenly stems ester, three (Lauryl Alcohol) ester, three (16 carbon alcohol) ester, naphthylamines, pentanoic, the Ursol D.
Prepare the method for above-mentioned a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material, may further comprise the steps:
(1) the active alkali magnesium sulfate crystal whisker pre-composition of preparation:
By weight part in the prescription alkali magnesium sulfate crystal whisker, coupling agent, processing aid are put into high mixer, by high pressure sprays fog equipment sour dilution evenly is sprayed onto in the mixture in the high mixer simultaneously, then carry out high-speed mixing, get active alkali magnesium sulfate crystal whisker pre-composition;
(2) composite manufacture:
After weight ratio mixes polypropylene, toughner and thermo-stabilizer in the prescription, in being the twin screw extruder of 35-50:1, length-to-diameter ratio carries out melting, mixing, dispersion, the active alkali magnesium sulfate crystal whisker pre-composition that again (1) is prepared adds from the side feeding of twin screw extruder, under 190-220 ℃ of temperature, plastify, by double-screw extruding pelletizing, just obtain active alkali formula magnesium sulfate crystal whisker modified polypropylene composite material again.
The preferred version of such scheme is, the temperature that described step (1) high speed is mixed is that 100-120 ℃, time are 5-10min.
The present invention compared with prior art has following some advantage:
1, alkali magnesium sulfate crystal whisker Reinforced Polypropylene of the present invention prepares in the polypropylene composite material because alkali magnesium sulfate crystal whisker has lower density, it develops to lightweight so be conducive to final engineering part, and be conducive to reduce the usage quantity of its material, reduce the use cost of material.
2, the alkali magnesium sulfate crystal whisker material of the present invention's use take preparing salt by working up seawater by product bittern as raw material, has the advantages such as wide material sources, environmental protection, and the energy-conserving and environment-protective that current national is advocated have very large meaning.
3, the alkali magnesium sulfate crystal whisker material that uses of the present invention, because of its have enhancings, fire-retardant, but the functions such as cigarette, filling are widely used in the modifying plastics material, make general-purpose plastics to the through engineering approaches future development, increase substantially use range and the degree of depth.
4, the alkali magnesium sulfate crystal whisker material that uses of the present invention, it is little to have a particle diameter, is easy to disperse in process of manufacture, less to the degree of wear of machine, effectively raises the work-ing life of twin-screw extrusion machine.
5, the present invention carries out surface activation process by silane coupling agent to alkali magnesium sulfate crystal whisker, strengthened the consistency of alkali magnesium sulfate crystal whisker and acrylic resin, compare with direct filling the such as existing breeze, fiber, be conducive to improve the Uniform Dispersion degree of alkali magnesium sulfate crystal whisker in matrix.
Embodiment:
The below provides embodiment so that the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, content still belongs to protection scope of the present invention to some nonessential improvement and the adjustment that the present invention makes to the person skilled in the art in this field according to the present invention.
All constitutive materials are existing commercially available prod in the embodiment of the invention, and all components are all in weight part, wherein:
Alkali magnesium sulfate crystal whisker be make take preparing salt by working up seawater by product bittern as raw material length-to-diameter ratio as 10-30, particle diameter as 0.5-4um.
Toughner is vinyl elastomerics or styrenic elastomerics, and the present invention preferentially selects polyethylene (PE), ethylene-octene polymkeric substance (POE), ethylene-propylene-butadiene terpolymer (EPDM).
Thermo-stabilizer is selected from least a in Hinered phenols, hindered amines, the phosphorous acid esters, wherein the Hinered phenols thermo-stabilizer has 2, three grades of butyl of 6--4-methylphenol, two (3, three grades of butyl of 5--4-hydroxy phenyl) thioether or four (β-(three grades of butyl of 3,5--4-hydroxy phenyl) propionic acid) pentaerythritol ester (1010) etc.; The phosphite type thermal stabilizing agent have three (2,4-di-tert-butyl-phenyl) phosphorous acid esters (168), three monooctyl esters, three the last of the ten Heavenly stems ester, three (Lauryl Alcohol) ester, three (16 carbon alcohol) ester; The hindered amines thermo-stabilizer has naphthylamines, pentanoic, Ursol D etc.
Coupling agent is silane coupling agent such as KH550, KH560, KH570, or a kind of among titante coupling agent NDZ-101, the NDZ-401.Preferred silane coupling agent KH550 of the present invention, KH560, KH570 model.
Processing aid is selected from least a in low molecular hydrocarbon, metal soap, stearic acid complex ester class and the amides processing aid.The present invention preferentially selects calcium stearate (Ca-St
2), ethylene bis stearamide (EBS), modification ethylene bis stearamide (TAF).
The acid dilution is at least a aqueous solution that forms with the water configuration in hydrochloric acid, sulfuric acid, the phosphoric acid, and the volume percent of described sour dilution is 0.5-2%.Selecting volume percent among the embodiment is 1% hydrochloric acid soln, 0.5% sulphuric acid soln, 1.5% phosphoric acid solution, or the mixture of 0.5% sulphuric acid soln and 0.5% hydrochloric acid soln.
In the present invention, following method is adopted in the preparation of active alkali magnesium sulfate crystal whisker modified polypropylene composite material:
The first step need prepare first active alkali magnesium sulfate crystal whisker pre-composition:
By weight part in the prescription alkali magnesium sulfate crystal whisker, coupling agent, processing aid are put into high mixer, by high pressure sprays fog equipment sour dilution evenly is sprayed onto in the mixture in the high mixer simultaneously, then carry out high-speed mixing 5-10min, temperature is 100-120 ℃, gets active alkali magnesium sulfate crystal whisker pre-composition;
Second step is composite manufacture:
After weight ratio mixes polypropylene, toughner and thermo-stabilizer in the prescription, in being the twin screw extruder of 35-50:1, length-to-diameter ratio carries out melting, mixing, dispersion, the active alkali magnesium sulfate crystal whisker pre-composition that again (1) is prepared adds from the side feeding of twin screw extruder, under 190-220 ℃ of temperature, plastify, by double-screw extruding pelletizing, just obtain active alkali formula magnesium sulfate crystal whisker modified polypropylene composite material again.
One, embodiment
Following specific embodiment 1-4 adopts above-mentioned preparation method to be prepared active alkali magnesium sulfate crystal whisker modified polypropylene composite material, and its raw material is also selected above-mentioned preferred kind.
Embodiment 1:
Co-polypropylene: 48 parts
Homo-polypropylene: 40 parts
Toughner POE:10 part
Processing aid TAF:0.7 part
Processing aid CaSt
2: 0.4 part
Silane coupling agent KH550: 0.3 part
Hydrochloric acid soln: 0.5 part
Thermo-stabilizer 1010:0.2 part
Thermo-stabilizer 168:0.2 part
Alkali magnesium sulfate crystal whisker: 10 parts
It is the 35:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, active alkali magnesium sulfate crystal whisker pre-composition is added from its side feeding, plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product again.
Embodiment 2:
Co-polypropylene: 42 parts
Homo-polypropylene: 28 parts
Toughner PE:8 part
Processing aid TAF:0.3 part
Processing aid EBS:0.4 part
Silane coupling agent KH560:0.4 part
Sulphuric acid soln: 0.4 part
Thermo-stabilizer 1010:0.3 part
Three grades of butyl of 2,6--4-methylphenol: 0.3 part
Alkali magnesium sulfate crystal whisker: 20 parts
It is the 40:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, active alkali magnesium sulfate crystal whisker pre-composition is added from its side feeding, plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product again.
Embodiment 3:
Co-polypropylene: 36 parts
Homo-polypropylene: 24 parts
Toughner POE:5 part
Processing aid TAF:0.1 part
Processing aid CaSt
2: 0.2 part
Silane coupling agent KH570:0.5 part
Phosphoric acid solution: 0.3 part
Two (three grades of butyl of 3,5--4-hydroxy phenyl) thioether: 0.5 part
Thermo-stabilizer 168:0.5 part
Alkali magnesium sulfate crystal whisker: 30 parts
It is the 50:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, active alkali magnesium sulfate crystal whisker pre-composition is added from its side feeding, plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product again.
Embodiment 4:
Co-polypropylene: 30 parts
Homo-polypropylene: 20 parts
Toughner EPDM:2 part
Processing aid EBS:0.1 part
Titante coupling agent NDZ-101:0.5 part
The mixing solutions of hydrochloric acid and sulfuric acid: 0.5 part
Three monooctyl esters: 0.1 part
Alkali magnesium sulfate crystal whisker: 40 parts
It is the 36:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, active alkali magnesium sulfate crystal whisker pre-composition is added from its side feeding, plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product again.
Two, comparative example
Because existing material for the preparation of inner and outer decorative parts of automobile mainly is to carry out filled modified polypropylene and make by adding conventional breeze such as calcium carbonate, talcum powder etc.In order to embody better advantage of the present invention, prepare contrast product according to prior art formula composition and preparation method thereof, its raw material forms to be prepared with reference to the component that provides among the present invention, and its preparation method is also with preparation method of the present invention, through mixing, granulation, be extruded into product.Concrete Comparative Examples is as follows:
Comparative Examples 1:
Co-polypropylene: 36 parts
Homo-polypropylene: 24 parts
Toughner POE:10 part
Processing aid TAF:0.3 part
Processing aid CaSt
2: 0.4 part
Thermo-stabilizer 1010:0.2 part
Thermo-stabilizer 168:0.2 part
The talcum powder extra large PT10:30 weight part that ends
It is the 36:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, processing aid, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, the extra large PT10 that again talcum powder ended adds from its side feeding, and plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product.
Comparative Examples 2:
Co-polypropylene: 36 weight parts
Homo-polypropylene: 24 weight parts
Toughner POE:10 weight part
Processing aid TAF:0.3 weight part
Processing aid CaSt
2: 0.4 weight part
Thermo-stabilizer 1010:0.2 weight part
Thermo-stabilizer 168:0.2 weight part
The big Xiang BX-1:30 weight part of calcium carbonate
It is the 36:1 twin screw extruder that present embodiment adopts length-to-diameter ratio, polypropylene, processing aid, toughner and thermo-stabilizer are carried out melting, mixing, dispersion in this forcing machine, the big Xiang BX-1 of calcium carbonate is added from its side feeding, plastifying also under 190-220 ℃ of temperature, extruding pelletization namely gets product again.
Three, simultaneous test test
The sample that makes among above-described embodiment 1-4 and the Comparative Examples 1-2 is injection molded into behind the standard batten to characterize according to GB according to unified technique tests, its concrete physical index is shown in following table 1,2:
Table 1: the main physical index of active alkali magnesium sulfate crystal whisker modified polypropylene composite material
| Project | Testing standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Alkali magnesium sulfate crystal whisker | / | 10 | 20 | 30 | 40 |
| Melt flow rate (MFR) g/10min | GB/T3682 | 13 | 18 | 19 | 21 |
| Shrinking percentage % | GB/T15585 | 1.4-1.6 | 1.2-1.4 | 1.1-1.3 | 0.5-0.7 |
| Density g/cm 3 | GB/T1033 | 0.96 | 1.01 | 1.05 | 1.17 |
| Tensile strength MPa | GB/T1040 | 24 | 24 | 24 | 25 |
| Flexural strength MPa | GB/T9341 | 33 | 34 | 36 | 38 |
| Modulus in flexure MPa | GB/T9341 | 1508 | 2090 | 2869 | 2998 |
| Notch shock KJ/m 2 | GB/T1843 | 9.1 | 12.5 | 15.2 | 10.3 |
| Heat-drawn wire ℃ (0.45Mpa) | GB/T16342 | 104 | 110 | 115 | 125 |
Data can be found out from table 1, and along with the alkali magnesium sulfate crystal whisker adding proportion increases, the flowability of matrix material, flexural strength, modulus in flexure and heat-drawn wire all increase, and the shock strength of embodiment 3 is maximum.
Table 2: embodiment 3 and Comparative Examples physical property contrast table
| Project | Testing standard | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| Melt flow rate (MFR) g/10min | GB/T3682 | 19 | 12 | 16 |
| Shrinking percentage % | GB/T15585 | 1.1-1.3 | 1.5-1.7 | 1.8-2.0 |
| Density g/cm 3 | GB/T1033 | 1.05 | 1.14 | 1.13 |
| Tensile strength MPa | GB/T1040 | 24 | 18 | 20 |
| Flexural strength MPa | GB/T9341 | 36 | 28 | 24 |
| Modulus in flexure MPa | GB/T9341 | 2869 | 2500 | 2200 |
| Notch shock KJ/m 2 | GB/T1843 | 15.2 | 8.2 | 10.3 |
| Heat-drawn wire ℃ (0.45Mpa) | GB/T16342 | 115 | 105 | 100 |
Data can be found out from table 2, alkali magnesium sulfate crystal whisker is compared with mineral fillers such as talcum powder, calcium carbonate in the modified polypropylene composite material, the shock strength of alkali magnesium sulfate reinforced polypropylene compound material is maximum, density is low, shrinking percentage is little, and tensile strength, flexural strength, heat-drawn wire and flowing property all are better than existing breeze filling strongthener, therefore, alkali magnesium sulfate crystal whisker has the value of actual development as a kind of novel strongthener.
Claims (10)
1. active alkali magnesium sulfate crystal whisker modified polypropylene composite material, it is characterized in that: the weight part of its constitutive material is:
Polypropylene: 50-88 part;
Alkali magnesium sulfate crystal whisker: 10-40 part;
Toughner: 2-10 part;
Processing aid: 0.1-1 part;
Coupling agent: 0.3-0.5 part;
Acid dilution: 0.3-0.5;
Thermo-stabilizer: 0.1-1 part.
2. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1 is characterized in that: described polypropylene is at least a in homopolymerization polypropylene, the Co-polypropylene, and its melting index is 10-25g/10min.
3. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: the length-to-diameter ratio of described alkali magnesium sulfate crystal whisker is that 10-30, particle diameter are 0.5-4um.
4. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: described toughner is vinyl elastomerics or styrenic elastomerics.
5. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: described processing aid is calcium stearate (Ca-St
2), at least a in the ethylene bis stearamide (EBS), modification ethylene bis stearamide (TAF).
6. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: described coupling agent is a kind of for being selected among silicane KH550, KH560, the KH570, or a kind of among titanate ester NDZ-101, the NDZ-40.
7. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: described sour dilution is at least a aqueous solution that forms with the water configuration in hydrochloric acid, sulfuric acid, the phosphoric acid, and the volume percent of described sour dilution is 0.5-2%.
8. a kind of active alkali magnesium sulfate crystal whisker modified polypropylene composite material according to claim 1, it is characterized in that: described thermo-stabilizer is selected from 2, three grades of butyl of 6--4-methylphenol, two (3, three grades of butyl of 5--4-hydroxy phenyl) thioether, four (β-(3, three grades of butyl of 5--4-hydroxy phenyl) propionic acid) pentaerythritol ester (1010), three (2,4-di-tert-butyl-phenyl) phosphorous acid esters (168) of phosphorous acid lipid, three monooctyl esters, three the last of the ten Heavenly stems ester, three (Lauryl Alcohol) ester, three (16 carbon alcohol) ester, naphthylamines, pentanoic, at least a in the Ursol D.
9. one kind prepares as claimed in claim 1 a kind of method of active alkali magnesium sulfate crystal whisker modified polypropylene composite material, it is characterized in that: may further comprise the steps:
(1) the active alkali magnesium sulfate crystal whisker pre-composition of preparation:
By weight part in the prescription alkali magnesium sulfate crystal whisker, coupling agent, processing aid are put into high mixer, by high pressure sprays fog equipment sour dilution evenly is sprayed onto in the mixture in the high mixer simultaneously, then carry out high-speed mixing, get active alkali magnesium sulfate crystal whisker pre-composition;
(2) composite manufacture:
After weight ratio mixes polypropylene, toughner and thermo-stabilizer in the prescription, in being the twin screw extruder of 35-50:1, length-to-diameter ratio carries out melting, mixing, dispersion, the active alkali magnesium sulfate crystal whisker pre-composition that again (1) is prepared adds from the side feeding of twin screw extruder, under 190-220 ℃ of temperature, plastify, by double-screw extruding pelletizing, just obtain active alkali formula magnesium sulfate crystal whisker modified polypropylene composite material again.
10. method according to claim 9 is characterized in that: the temperature that described step (1) high speed is mixed is that 100-120 ℃, time are 5-10min.
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| CN113754969B (en) * | 2021-10-08 | 2022-11-01 | 福建亚通新材料科技股份有限公司 | HDPE/PVC blending modified material |
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| CN119161662A (en) * | 2024-06-06 | 2024-12-20 | 江苏乾涌控股有限公司 | A high-toughness and high-rigidity polypropylene composite material and preparation method thereof |
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