CN116082753A - Flame-retardant short glass fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
Flame-retardant short glass fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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- CN116082753A CN116082753A CN202211730134.XA CN202211730134A CN116082753A CN 116082753 A CN116082753 A CN 116082753A CN 202211730134 A CN202211730134 A CN 202211730134A CN 116082753 A CN116082753 A CN 116082753A
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- 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 title claims abstract description 78
- 239000003063 flame retardant Substances 0.000 title claims abstract description 74
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 51
- -1 polypropylene Polymers 0.000 title claims abstract description 49
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 46
- 239000003365 glass fiber Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 26
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 7
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 7
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 6
- 239000005373 porous glass Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 239000000835 fiber Substances 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/14—Copolymers of propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a flame-retardant short glass fiber reinforced polypropylene composite material and a preparation method thereof, wherein the flame-retardant short glass fiber reinforced polypropylene composite material is prepared from the following components in parts by weight: 55-65 parts of base material polypropylene, 10-20 parts of glass fiber, 10-15 parts of composite flame retardant unit, 1-1.5 parts of toner, 1-2 parts of antioxidant and 3-4 parts of graft. Compared with common same-grade flame-retardant reinforced polypropylene in the market, the short glass fiber reinforced polypropylene composite material prepared by the invention has the advantages that the design and production of a general flame-retardant unit are carried out, the use amount of a flame retardant of the material is effectively reduced on the premise of consistent flame retardant property of the material, the use cost of the flame-retardant short fiber reinforced material is greatly reduced, the carbon emission in the production process is effectively reduced, and the short glass fiber reinforced polypropylene composite material can be widely applied to the field of injection-molded parts of automobiles.
Description
Technical Field
The invention relates to the technical field of polypropylene materials, in particular to a low-cost light flame-retardant short glass fiber reinforced polypropylene composite material and a preparation method thereof. The material is suitable for manufacturing automobile seats, interior peripheral parts and the like.
Technical Field
The plastic industry has been growing rapidly for about 30 years, and the application field of the plastic industry has been related to the aspects of society, and the plastic industry plays an important role in people's transportation. With the proposal of energy conservation and carbon reduction, a large number of new energy vehicle enterprises rapidly rise in the field of low-carbon travel, and benefit from the technical revolution of clean energy on one hand and from the development of material technology on the other hand. China is a army of new energy automobiles, and the requirement of enterprises of the new energy automobiles in China on lightweight materials is a leading global. How to realize the weight reduction of the whole car and reduce the production cost are problems facing to various large modified material enterprises in future. The fiber reinforced plastic is a common composite material, is one of important materials appearing under the concept of plastic steel substitute, and in the large environment of carbon reduction production nowadays, the requirement of a new energy host factory is hardly met only by keeping the traditional high mechanical property, and the material is required to have other specific functionalities. The composite material which can meet a plurality of use requirements is an effective means for realizing the reduction of energy consumption and cost of plastics in the automobile industry, improving benefits and achieving the aim of carbon neutralization.
The short fiber reinforced material has wide application in automobile parts, is widely applied to various supporting parts, interior part frameworks and the like, and is increasingly applied to cabin interior parts through part structural design and optimization of injection molding technology. For the consideration of riding safety, the interior material of the automobile cabin needs to have certain flame-retardant capability on the basis of certain mechanical properties. Most common flame-retardant materials are flame-retardant PP and flame-retardant ABS, and the mechanical properties and the production cost of the two materials have certain irreconcilability. The short fiber reinforced material has unique advantages based on the three aspects of balancing weight reduction, maintaining mechanical properties and flame retardant properties. However, short fiber reinforced polypropylene has its own drawbacks to be solved. On one hand, the flame-retardant short fiber material has higher production cost, and the aim of effectively replacing and reducing the cost is difficult to achieve. On the other hand, the common PP flame-retardant system is limited by a production mode, the dispersion of the common PP flame-retardant system in granules is often not uniform enough, the flame-retardant effect is insufficient, and the problem is particularly obvious when different flame-retardant systems act cooperatively, so that the common flame-retardant short fiber at present adopts a single flame-retardant system. These technical problems have caused great problems for popularization of the use of the short fiber flame-retardant material.
In the production process of the low-cost lightweight flame-retardant short glass fiber reinforced polypropylene composite material, the invention innovates both the product formula and the production process from the production requirement of enterprises. The formula changes the mixing mode of the traditional glass fiber material and the single flame-retardant master batch, firstly prepares the composite flame-retardant unit, and then takes the unit as a part of raw materials to be directly added at the front end of production. The flame-retardant component adopts a mode of synergistic effect of an intumescent flame-retardant system and an organosilicon flame-retardant system, and in order to solve the dispersion problem of the two systems, the flame-retardant unit is prepared by innovatively adopting the mode that MMT is taken as a carrier to be adsorbed in porous glass microspheres. Compared with a material system short fiber filler, the porous glass microsphere has larger specific surface area and obviously reduced cost on the premise of keeping the same level of performance. The addition of the composite flame retardant unit can effectively solve the problem of decomposition of the flame retardant, and simultaneously, the synchronous extrusion is stable and uniform, which is also beneficial to closing of the carbon layer of the intumescent flame retardant in the system, and the flame retardant efficiency is enhanced.
Disclosure of Invention
The invention aims to solve the technical problems that the production cost of the traditional flame-retardant short glass fiber reinforced polypropylene material is too high and the flame-retardant effect is uneven. The cost-saving flame-retardant short glass fiber reinforced polypropylene composite material is provided:
in order to solve the technical problems, the invention adopts the following technical scheme:
a flame-retardant short glass fiber reinforced polypropylene composite material is characterized in that: the adhesive comprises the following components in parts by weight: 55-65 parts of base material polypropylene, 10-20 parts of glass fiber, 10-15 parts of composite flame retardant unit, 1-1.5 parts of toner, 1-2 parts of antioxidant and 3-4 parts of graft.
The base material polypropylene is low melt index copolymerized polypropylene, and the MFR is less than or equal to 25.
The composite flame-retardant unit is as follows: the pore diameter of the organic silicon modified porous glass microsphere is more than or equal to 5 mu m, the particle diameter is more than or equal to 50 mu m, and the organic modified sodium montmorillonite and the flame retardant component are adsorbed on the surface and the inside of the porous glass microsphere.
The montmorillonite is one of sodium hexadecyl sulfonate modified sodium montmorillonite, acid montmorillonite, alkali montmorillonite and silane coupling agent modified sodium montmorillonite; the flame retardant component is compounded by ammonium polyphosphate (APP), pentaerythritol and melamine.
The graft is at least one of PP-g-MAH maleic anhydride graft, KH550 silane coupling agent, KH570 silane coupling agent and acrylic grafted PP.
The glass fiber is alkali-free glass fiber chopped yarn: the diameter of the monofilament is 10-14 mu m.
The antioxidant is at least two of general 168, 619F,1010, 1076, 1035 and DSTP, 1010.
The toner is carbon black.
The preparation method of the flame-retardant short glass fiber reinforced polypropylene composite material is characterized by comprising the following steps of:
(1) Preparing flame-retardant modified MMT: putting sodium-based MMT into ethanol and cyclohexane blend solution, refluxing and stirring for 24 hours, and adding KH570 silane coupling agent at a constant speed according to a weight ratio of 1:1 during the refluxing and stirring to obtain silane coupling agent modified MMT; cleaning for more than 3 times by using a solution to remove residual coupling agent, re-blending, dissolving a small amount of melamine in ammonium polyphosphate and pentaerythritol, slowly adding MMT modified by the silane coupling agent, refluxing, cleaning and drying to obtain flame-retardant modified MMT;
(2) Stirring the flame-retardant modified MMT with deionized water until the flame-retardant modified MMT is completely swelled, adding the porous hollow glass, soaking for 10 hours to ensure sufficient adsorption, and screening out the sufficiently adsorbed glass beads to be used as a flame-retardant unit;
(3) Mixing and stirring raw materials of polypropylene, an antioxidant and toner at a high speed according to a proportion;
(4) And (3) uniformly mixing the materials in the step (3), feeding the mixture into a double-screw extruder, wherein the processing temperature is 200-240 ℃, the rotating speed of a main machine is 300-600rpm, adding an ultrasonic dispersing device at the position of a stirring machine head, and applying ultrasonic waves with fixed frequency (20-40 Hz) to the position of the machine head. Adding chopped continuous yarn alkali-free glass fiber into a feeding port at the first side of the front section, and adding a vacuum pumping system in the stirring process; adding the flame-retardant unit into a second side feeding port positioned at the rear section for stirring;
(5) The segmented extrusion devices are respectively provided with a front segment 200 ℃, a middle segment 220 ℃ and a tail segment 230 ℃, and then are cooled by a water tank and granulated by a granulator to prepare reinforced polypropylene granules with the length of 2-4mm, and the ash content is 20-30%.
Compared with common same-grade flame-retardant reinforced polypropylene in the market, the short glass fiber reinforced polypropylene composite material prepared by the invention has the advantages that the design and production of a general flame-retardant unit are carried out, the use amount of a flame retardant of the material is effectively reduced on the premise of consistent flame retardant property of the material, the use cost of the flame-retardant short fiber reinforced material is greatly reduced, the carbon emission in the production process is effectively reduced, and the short glass fiber reinforced polypropylene composite material can be widely applied to the field of injection-molded parts of automobiles.
Detailed Description
The following examples are presented to further illustrate the invention in connection with the practice thereof, but are not intended to limit the invention in any manner.
The compositions and the contents of the components contained in the comparative examples and the examples according to the invention are shown in the following Table 1, and the compositions and the contents of the formulations of the examples and the comparative examples are shown in the following Table 1
The procedure was as in the examples above:
(1) Preparing flame-retardant modified MMT: and (3) putting the sodium-based MMT into the ethanol and cyclohexane blend solution, refluxing and stirring for 24 hours, and adding the KH570 silane coupling agent at a constant speed according to the weight ratio of 1:1 during the refluxing and stirring to obtain the silane coupling agent modified MMT. And (3) cleaning the mixture for more than 3 times by using a solution to remove the residual coupling agent, re-blending the mixture, dissolving ammonium polyphosphate, a small amount of pentaerythritol, melamine and polysilane, slowly adding the MMT modified by the silane coupling agent, and carrying out reflux, cleaning and drying to obtain the flame-retardant modified MMT.
(2) And stirring the flame-retardant modified MMT with deionized water until the flame-retardant modified MMT is completely swelled, adding the porous hollow glass, soaking for 10 hours to ensure sufficient adsorption, and screening out the sufficiently adsorbed glass beads to be used as a flame-retardant unit.
(3) Mixing and stirring raw materials of polypropylene, an antioxidant and toner at a high speed according to a proportion.
(4) And (3) uniformly mixing the materials in the step (3), feeding the mixture into a double-screw extruder, wherein the processing temperature is 200-240 ℃, the rotating speed of a main machine is 300-600rpm, adding an ultrasonic dispersing device at the position of a stirring machine head, and applying ultrasonic waves with fixed frequency (20-40 Hz) to the position of the machine head. The chopped continuous yarn alkali-free glass fiber is added into a feeding port at the first side of the front section, and a vacuum pumping system is added in the stirring process. The flame-retardant unit is added into a second side feeding port positioned at the rear section for stirring.
(5) The sectional extrusion devices are respectively at the front section of 200 ℃, the middle section of 220 ℃, the tail section of 230 ℃, and then are cooled by a water tank and granulated by a granulator to prepare reinforced polypropylene granules with the length of 2-4mm, and the ash content is 30%;
the preparation of comparative example 1 is according to table 1:
(1) Mixing and stirring the raw materials of polypropylene, a compatilizer, an antioxidant and carbon black master batch at a high speed according to a proportion.
(2) And (3) uniformly mixing the materials in the step (1), feeding the mixture into a double-screw extruder, wherein the processing temperature is 200-240 ℃, the rotating speed of a main machine is 300-600rpm, adding an ultrasonic dispersing device at the position of a stirring machine head, and applying ultrasonic waves with fixed frequency (20-40 Hz) to the position of the machine head. And adding the chopped continuous yarn alkali-free glass fiber into the side feeding port, and adding a vacuum pumping system in the stirring process.
(3) The sectional extrusion devices are respectively 200 ℃,220 ℃,220 ℃,230 ℃, and then are cooled by a water tank and pelletized by a pelletizer to prepare reinforced polypropylene pellets with the length of 2-4mm, wherein the weight content of fibers is 30%;
according to table 1 comparative examples 2, 3:
(1) The raw materials of polypropylene, compatilizer, antioxidant, carbon black master batch and flame retardant components are mixed and stirred at a high speed according to a proportion.
(2) And (3) uniformly mixing the materials in the step (1), feeding the mixture into a double-screw extruder, wherein the processing temperature is 200-240 ℃, the rotating speed of a main machine is 300-600rpm, adding an ultrasonic dispersing device at the position of a stirring machine head, and applying ultrasonic waves with fixed frequency (20-40 Hz) to the position of the machine head. And adding the chopped continuous yarn alkali-free glass fiber into the side feeding port, and adding a vacuum pumping system in the stirring process.
(3) The sectional extrusion devices are respectively 200 ℃,220 ℃,220 ℃,230 ℃, and then are cooled by a water tank and cut into granules by a granulator to prepare reinforced polypropylene granules with the length of 2-4mm, and the weight content of the fiber is 30 percent
The flame retardant standard of the invention adopts the UL-94 vertical burning grade standard.
Table 2 results of performance tests for examples and comparative examples
As can be seen from the table, compared with the flame-retardant fiber reinforced polypropylene produced by the conventional production method, the flame-retardant polypropylene has obviously reduced addition amount of the flame retardant when meeting the same flame-retardant grade requirement. When the flame retardant and the like of the material are kept consistent with the original addition amount, the flame retardant and the like of the material are obviously improved, and the mechanical properties are at the same level. The preparation method of the new material utilizes the high specific surface area of the glass beads to ensure that the flame retardant components are more uniform, ensures the synergistic effect of different systems, and reduces the overall use amount. This approach facilitates low carbon production of the flame retardant material; the cost of the porous microbead is partially reduced compared with that of the traditional short fiber, which is beneficial to reducing the use cost in the subsequent use.
The above examples are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (9)
1. A flame-retardant short glass fiber reinforced polypropylene composite material is characterized in that: the adhesive comprises the following components in parts by weight: 55-65 parts of base material polypropylene, 10-20 parts of glass fiber, 10-15 parts of composite flame retardant unit, 1-1.5 parts of toner, 1-2 parts of antioxidant and 3-4 parts of graft.
2. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the base material polypropylene is low melt index copolymerized polypropylene, and the MFR is less than or equal to 25.
3. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the composite flame-retardant unit is as follows: the pore diameter of the organic silicon modified porous glass microsphere is more than or equal to 5 mu m, the particle diameter is more than or equal to 50 mu m, and the organic modified sodium montmorillonite and the flame retardant component are adsorbed on the surface and the inside of the porous glass microsphere.
4. A flame retardant short glass fiber reinforced polypropylene composite according to claim 3, wherein: the montmorillonite is one of sodium hexadecyl sulfonate modified sodium montmorillonite, acid montmorillonite, alkali montmorillonite and silane coupling agent modified sodium montmorillonite; the flame retardant component is compounded by ammonium polyphosphate (APP), pentaerythritol and melamine.
5. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the graft is at least one of PP-g-MAH maleic anhydride graft, KH550 silane coupling agent, KH570 silane coupling agent and acrylic grafted PP.
6. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the glass fiber is alkali-free glass fiber chopped yarn: the diameter of the monofilament is 10-14 mu m.
7. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the antioxidant is at least two of general 168, 619F,1010, 1076, 1035 and DSTP, 1010.
8. The flame-retardant short glass fiber reinforced polypropylene composite material according to claim 1, wherein: the toner is carbon black.
9. The method for preparing the flame-retardant short glass fiber reinforced polypropylene composite material according to any one of claims 1 to 8, comprising the following steps:
(1) Preparing flame-retardant modified MMT: putting sodium-based MMT into ethanol and cyclohexane blend solution, refluxing and stirring for 24 hours, and adding KH570 silane coupling agent at a constant speed according to a weight ratio of 1:1 during the refluxing and stirring to obtain silane coupling agent modified MMT; cleaning for more than 3 times by using a solution to remove residual coupling agent, re-blending, dissolving a small amount of melamine in ammonium polyphosphate and pentaerythritol, slowly adding MMT modified by the silane coupling agent, refluxing, cleaning and drying to obtain flame-retardant modified MMT;
(2) Stirring the flame-retardant modified MMT with deionized water until the flame-retardant modified MMT is completely swelled, adding the porous hollow glass, soaking for 10 hours to ensure sufficient adsorption, and screening out the sufficiently adsorbed glass beads to be used as a flame-retardant unit;
(3) Mixing and stirring raw materials of polypropylene, an antioxidant and toner at a high speed according to a proportion;
(4) And (3) uniformly mixing the materials in the step (3), feeding the mixture into a double-screw extruder, wherein the processing temperature is 200-240 ℃, the rotating speed of a main machine is 300-600rpm, adding an ultrasonic dispersing device at the position of a stirring machine head, and applying ultrasonic waves with fixed frequency (20-40 Hz) to the position of the machine head. Adding chopped continuous yarn alkali-free glass fiber into a feeding port at the first side of the front section, and adding a vacuum pumping system in the stirring process; adding the flame-retardant unit into a second side feeding port positioned at the rear section for stirring;
(5) The segmented extrusion devices are respectively provided with a front segment 200 ℃, a middle segment 220 ℃ and a tail segment 230 ℃, and then are cooled by a water tank and granulated by a granulator to prepare reinforced polypropylene granules with the length of 2-4mm, and the ash content is 20-30%.
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| CN105131430A (en) * | 2015-10-15 | 2015-12-09 | 贵州大学 | Halogen-free flame-retardant long-glass-fiber reinforced polypropylene composite |
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| CN105131430A (en) * | 2015-10-15 | 2015-12-09 | 贵州大学 | Halogen-free flame-retardant long-glass-fiber reinforced polypropylene composite |
| CN112940439A (en) * | 2021-03-02 | 2021-06-11 | 宁波福尔达智能科技有限公司 | Flame-retardant ABS composite material and preparation process thereof |
| CN114479288A (en) * | 2021-12-29 | 2022-05-13 | 上海普利特复合材料股份有限公司 | Flame-retardant long glass fiber reinforced polypropylene composite material for automobile and preparation method thereof |
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