CN105482255A - Environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material and preparation method thereof - Google Patents
Environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
- B29B9/14—Making granules characterised by structure or composition fibre-reinforced
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K5/02—Halogenated hydrocarbons
- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
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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
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1535—Five-membered rings
- C08K5/1539—Cyclic anhydrides
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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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses an environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material and a preparation method thereof. The environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material comprises 10-50% of long glass fiber which is arranged in parallel to the particle length, 35-70% of modified polypropylene resin and 15-30% of compound flame retardant. The modified polypropylene resin is prepared by the following steps: adding assistants into the existing commercial polypropylene resin to perform modification, and carrying out reaction extrusion by using a double screw extruder or any other melt impregnator. The environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material has the advantages of low material cost, simple processing technique and favorable product properties, can easily implement large-scale production and processing, and especially has favorable forming effect and flame-retardant characteristic for vehicle parts with high requirements for flame retardancy. The product disclosed by the invention has favorable mechanical properties, such as favorable tensile strength, bending strength and impact resistance. The environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material also has the characteristics of low smell, low VOC (volatile organic compound) and the like.
Description
Technical field
The present invention relates to a kind of polypropylene composite material, relate in particular to a kind of environmental protection flame retardant, long glass fiber reinforced polypropylene composite material and manufacture method thereof.
Background technology
Along with automotive industry fast development, the per capita rate of passenger car is climbed to a higher point successively, and incident in this is the demand growing to automotive material, also more and more higher to the requirement of material each side.Especially along with electronic, and the exploitation of hybrid electric vehicle and putting goods on the market, high-weatherability is proposed for all multiple components such as battery cell cases, the requirement of high flame retardant.On market in automobile-used interior material, long glass fiber-reinforced polypropylene materials has good rigid-tough balance, and can meet the mechanical property requirements of component in more car, thermotolerance is good; Meanwhile, after flame-retardant modified, still under maintenance relatively preferably performance prerequisite, cheap price can be realized, therefore there is the very large market development and application prospect.
Long glass fiber reinforced thermoplastic resin is a kind of glass fibre parallel arrangement and its length thermoplastic resin identical with resin granular material length in particle.Compared with strengthening thermoplastic resin with conventional staple, there are more excellent mechanical property, fatigue performance, creep-resistant property, weather alternation etc.; Particularly the shock resistance of material is very excellent.
But, in this material preparation technology, because processing temperature is higher, fire retardant usually can be made to degrade in the process of glass melt impregnation, thus flame retardant effect is deteriorated, and the homogeneity of dipping is also a large difficult point.Although when using thermosetting resin (as epoxy resin or polyester) to carry out impregnation of fibers, difficulty is not too large, because these thermosetting resins are often liquid or solution before curing.Have the thermoplastic resin of quite high fusing point with under room temperature for solid, due to higher melt temperature and very high crystallization rate, the abundant dipping of fiber is more difficult.Therefore, the resin matrix selecting high temperature current downflow characteristic comparatively to mate and fire retardant, add lubricant under necessary condition, be also in material preparation process outbalance a bit.
All the time, the long glass fiber reinforced material of environmental protection flame retardant system, the high temperature required due to its machining, the dispersiveness of glass and the requirement of flame-retarding characteristic, carry out in the industry the manufacture of this field product and produce few.One of its potential cause is fire retardant fancy price, and as everyone knows, in the plastic, bromide fire retardant occupies absolute predominance in organic fire-resisting system, although " blame " multiterminal are difficult to have other fire retardant systems to replace in environmental issue always.Although non-halogen flame retardant has, addition is few, the high and low cigarette of flame retarding efficiency, low toxicity, the advantage such as of many uses, but its price allows most of user hang back, therefore, when carrying out starting material exploitation, just these factors should be taken in and accept or reject, reduce subsequent forming and use cost.Although the present invention use TDE and fire retarding synergist be Halogen sex flame retardant, it does not belong to polybromodiphenyl ether, absolutely not generation PBDD or PBDF in burning, because of but a environment friendly flame retardant.Relative low price, can adapt to the needs of large-scale production, have comparatively wide market application foreground simultaneously.
Summary of the invention
The object of this invention is to provide environmental protection flame retardant, the long glass fiber reinforced polypropylene material of simple, the every excellent in mechanical performance of a kind of preparation technology, to improve the flame-retarding characteristic of material, do not affect the original mechanical property of material simultaneously, lowly distribute the PP matrix material with excellent combination property, meet the basic technology performance requriements as material for car interior trim parts.
Another object of the present invention is to provide the preparation method of above-mentioned environmental protection flame retardant, long glass fiber reinforced polypropylene material.
The present invention seeks to realize like this:
A kind of environmental protection flame retardant, long glass fiber reinforced polypropylene composite material, its composition by weight percentage, comprises 10 ~ 50% long glass fibress, the modified polypropylene resin of 35 ~ 70%, 15 ~ 30% compound flame redundant.
Described modified polypropylene resin carries out reactive extrursion preparation to existing commercial acrylic resin by melt kneading equipment such as twin screws, and described modified polypropylene resin includes the raw material of following weight percent meter:
Wherein,
Described compound flame redundant is mixed by phosphonium flame retardant phenyl hypo-aluminum orthophosphate, TDE and fire retarding synergist.Described phenyl hypo-aluminum orthophosphate: TDE: fire retarding synergist=2:3-4:1-2.
The melting index of described acrylic resin is 30 ~ 60g/10min.
Described black masterbatch is the black masterbatch of particle diameter between 0.5mm-3mm.
The method of above-mentioned environmental protection flame retardant, long glass fiber reinforced polypropylene composite material, its step is as follows:
(1) preparation band modified polypropylene resin: use two component weighing balance, acrylic resin and compound flame redundant is added at main opening for feed, maleic anhydride and l is added at side direction opening for feed, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB), black masterbatch, enters twin screw extruder after mixing of materials is even; Extruding processing temperature is 100 ~ 240 DEG C, and engine speed is 200 ~ 500rpm.
(2) prepare long glass fiber reinforced polypropylene material: melt modification acrylic resin melt impregnation continuous long glass fiber bundle, impregnation processability temperature is 240 ~ 260 DEG C, adopts pultrude process to prepare long glass fiber reinforced polypropylene material.
Described mixture enters dipping die head from forcing machine, evenly after the trailed continuous glass fibre of parcel dipping, becomes length to be the long glass fiber reinforced polypropylene material particle of 10 ~ 15mm through tank cooling, dicing machine pelletizing.
The present invention has following beneficial effect: lower cost for material, and complete processing is simple, and product properties is excellent, and easy large-scale production processing, especially for the vehicle component that flame-retardancy requirements is high, has good molding effect and flame-retarding characteristic; Goods of the present invention have good mechanical property, as good stretching, flexural strength and erosion-resisting characteristics; Also there is good low smell simultaneously, the characteristics such as low VOC.
Embodiment
Further illustrate the present invention below by embodiment and comparative example, do not violating under aim of the present invention, the present invention should be not limited to the content that following experimental example is specifically expressed.
Embodiment raw materials is as follows:
Acrylic resin 1 (PP-l): melting index 50, test condition 230 DEG C of * 2.16kg;
Acrylic resin 2 (PP-2): melting index 70, test condition 230 DEG C of * 2.16kg;
Flame-retardant system formula 1 (A1): phenyl hypo-aluminum orthophosphate: TDE: fire retarding synergist=2:3:2;
Flame-retardant system formula 2 (A2): phenyl hypo-aluminum orthophosphate: TDE: fire retarding synergist=2:4:1;
Continuous glass fibre; PPG company ECI7-4588;
L, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB): analytical pure, commercially available.
Maleic anhydride: technical grade, commercially available.
Black masterbatch: particle diameter 3mm, commercially available.
Product performance testing method:
Melt mass flow index (melting index): by ISO1133 method, at 230 DEG C, tests under 2.16kg load.
Tensile property: by ISO527 method, draw speed 5mm/min.
Bending property: by ISO178 method, trial speed 2mm/min.
Notched Izod impact strength: by ISO179 method, the thick sample of 4mm.
Combustioncharacteristics: by UL94 method, 1.6mm.
Total carbon VOC tests: test according to PV3341 standard GC-MS, and test value≤50 μ gC/g is qualified.
Embodiment 1
Use TE-65 (length-to-diameter ratio L/D=48) twin screw extruder with side direction spout, 1106 grams of acrylic resin PP-1 and 400 gram fire retardant A1 is added at main opening for feed, 20 grams of black masterbatch are added at side opening for feed, 4 grams of l, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB)s and 70 grams of maleic anhydrides.Processing temperature (from spout to die head) is respectively: 150 DEG C, 190 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, engine speed is 350rpm.
Pultrude process is adopted through the mixture of forcing machine frit reaction and continuous glass fibre, impregnation processability temperature is 240 DEG C, by cooling and dicing after dipping head, make fibre weight percentage composition and be 20% and its length long glass fiber reinforced PP particulate material identical with resin granular material length, adopt injection moulding machine preparation standard mechanical test sample, test result is in table 1.
Embodiment 2
Use is with TE-65 (length-to-diameter ratio L/D=48) twin screw extruder of side direction spout, 1108 grams of acrylic resin PP-2 and 400 gram fire retardant A1 is added at main opening for feed, 20 grams of black masterbatch are added at side opening for feed, 2 grams of l, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB)s and 70 grams of maleic anhydrides.Processing temperature (from spout to die head) is respectively: 150 DEG C, 190 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, engine speed is 350rpm.
Pultrude process is adopted through the mixture of forcing machine frit reaction and continuous glass fibre, impregnation processability temperature is 240 DEG C, by cooling and dicing after dipping head, make fibre weight percentage composition and be 20% and its length long glass fiber reinforced PP particulate material identical with resin granular material length, adopt injection moulding machine preparation standard mechanical test sample, test result is in table 1.
Embodiment 3
Use TE-65 (length-to-diameter ratio L/D=48) twin screw extruder with side direction spout, add 1010 grams of acrylic resin PP-1 and 500 gram fire retardant A2 at main opening for feed, add 20 grams of black masterbatch at side opening for feed, 70 grams of maleic anhydrides.Processing temperature (from spout to die head) is respectively: 150 DEG C, 190 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, engine speed is 350rpm.
Pultrude process is adopted through the mixture of forcing machine frit reaction and continuous glass fibre, impregnation processability temperature is 240 DEG C, by cooling and dicing after dipping head, make fibre weight percentage composition and be 20% and its length long glass fiber reinforced PP particulate material identical with resin granular material length, adopt injection moulding machine preparation standard mechanical test sample, test result is in table 1.
Embodiment 4
Use TE-65 (length-to-diameter ratio L/D=48) twin screw extruder with side direction spout, 801 grams of acrylic resin PP-2 and 500 gram fire retardant A1 is added at main opening for feed, 17 grams of black masterbatch are added at side opening for feed, 2 grams of l, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB)s and 80 grams of maleic anhydrides.Processing temperature (from spout to die head) is respectively: 150 DEG C, 190 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, engine speed is 350rpm.
Pultrude process is adopted through the mixture of forcing machine frit reaction and continuous glass fibre, impregnation processability temperature is 240 DEG C, by cooling and dicing after dipping head, make fibre weight percentage composition and be 30% and its length long glass fiber reinforced PP particulate material identical with resin granular material length, adopt injection moulding machine preparation standard mechanical test sample, test result is in table 1.
Embodiment 5
Use TE-65 (length-to-diameter ratio L/D=48) twin screw extruder with side direction spout, 801 grams of acrylic resin PP-2 and 500 gram fire retardant A2 is added at main opening for feed, 17 grams of black masterbatch are added at side opening for feed, 2 grams of l, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB)s and 80 grams of maleic anhydrides.Processing temperature (from spout to die head) is respectively: 150 DEG C, 190 DEG C, 200 DEG C, 220 DEG C, 240 DEG C, 240 DEG C, 240 DEG C, 245 DEG C, engine speed is 350rpm.
Pultrude process is adopted through the mixture of forcing machine frit reaction and continuous glass fibre, impregnation processability temperature is 240 DEG C, by cooling and dicing after dipping head, make fibre weight percentage composition and be 30% and its length long glass fiber reinforced PP particulate material identical with resin granular material length, adopt injection moulding machine preparation standard mechanical test sample, test result is in table 1.
Table 1: the performance test results
As seen from the above table, in the long glass fiber-reinforced polypropylene materials of identical melting means PP material preparation, the flame-retardant system of different ratio can make material mechanical performance be subject to the fluctuation impact of certain limit; In different flame-retardant system, the ratio of compound flame redundant is different, can make flame retardant effect generation noticeable change.Along with the melting means of PP base-material changes, the mechanical property also corresponding change of obtained long glass fiber reinforced material, melting means becomes large, the material of identical glass fiber content, and toughness can decrease; In the base-material of melting means 50 and 70, melting means be 50 toughness of material better.
The present invention is by adopting twin screw extruder to carry out reactive extrursion to existing commercial acrylic resin, prepare the modified polypropene that mobility is moderate, in this, as resin matrix, adopt melt impregnation method, pultrusion impregnation technology has prepared long glass fiber reinforced polypropylene material.Compared with prior art, the present invention has following beneficial effect: lower cost for material, and complete processing is simple, and product properties is excellent, and easy large-scale production processing, especially for the vehicle component that flame-retardancy requirements is high, has good molding effect and flame-retarding characteristic; Goods of the present invention have good mechanical property, as good stretching, flexural strength and erosion-resisting characteristics; Also there is good low smell simultaneously, the characteristics such as low VOC.
The moulded parts obtained by the present invention can be widely used in the part with flame-retardancy requirements in automotive industry and other field of traffic; Be applied to Communication Equipment and equipment, consumer electronics, household electrical appliances, mechanical battery cell case material and annex etc., market application foreground is wide.
Claims (7)
1. an environmental protection flame retardant, long glass fiber reinforced polypropylene composite material, it is characterized in that: by weight percentage, comprise the long glass fibres that 10 ~ 50% modes parallel with particle length arrange, the modified polypropylene resin of 35 ~ 70%, 15 ~ 30% compound flame redundant; Described modified polypropylene resin comprises the raw material of following weight percent meter:
2. a kind of environmental protection flame retardant according to claim 1, long glass fiber reinforced polypropylene composite material, is characterized in that: described compound flame redundant is mixed by phosphonium flame retardant phenyl hypo-aluminum orthophosphate, TDE and fire retarding synergist.
3. a kind of environmental protection flame retardant according to claim 2, long glass fiber reinforced polypropylene composite material, is characterized in that: described phenyl hypo-aluminum orthophosphate: TDE: fire retarding synergist=2:3-4:1-2.
4. environmental protection flame retardant according to claim 1, long glass fiber reinforced polypropylene composite material, is characterized in that: the melting index of described acrylic resin is 30 ~ 60g/10min.
5. environmental protection flame retardant according to claim 1, long glass fiber reinforced polypropylene composite material, is characterized in that: described black masterbatch is the black masterbatch of particle diameter between 0.5mm-3mm.
6. prepare a method for environmental protection flame retardant described in claim 1, long glass fiber reinforced polypropylene composite material, it is characterized in that: its step is as follows:
(1) preparation band modified polypropylene resin: use two component weighing balance, acrylic resin and compound flame redundant is added at main opening for feed, maleic anhydride and l is added at side direction opening for feed, 4-(dual-tert-butyl peroxide) diisopropylbenzene(DIPB), black masterbatch, enters twin screw extruder after mixing of materials is even; Extruding processing temperature is 100 ~ 240 DEG C, and engine speed is 200 ~ 500rpm.
(2) prepare long glass fiber reinforced polypropylene material: melt modification acrylic resin melt impregnation continuous long glass fiber bundle, impregnation processability temperature is 240 ~ 260 DEG C, adopts pultrude process to prepare long glass fiber reinforced polypropylene material.
7. the preparation method of polypropylene composite material according to claim 6; it is characterized in that: mixture enters dipping die head from forcing machine; after the trailed continuous glass fibre of even parcel dipping, length is become to be the long glass fiber reinforced polypropylene material particle of 10 ~ 15mm through tank cooling, dicing machine pelletizing.
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| CN106589579A (en) * | 2016-10-27 | 2017-04-26 | 上海普利特复合材料股份有限公司 | High-size-stability long glass fiber reinforced polypropylene composite material and preparation method thereof |
| CN106926380A (en) * | 2017-04-11 | 2017-07-07 | 四川福思达生物技术开发有限责任公司 | A kind of production technology and its production system of hypo-aluminum orthophosphate nylon66 fiber |
| CN107910466A (en) * | 2017-11-09 | 2018-04-13 | 江苏澳盛复合材料科技有限公司 | New-energy automobile fibre reinforced composites Battery case and its processing method |
| CN108192204A (en) * | 2017-12-27 | 2018-06-22 | 重庆普利特新材料有限公司 | A kind of flame-retardant long glass fiber reinforced polypropylene composite material and its manufacturing method of low smoke density |
| CN110183777A (en) * | 2019-05-23 | 2019-08-30 | 浙江汇晶新材料有限公司 | Based on long glass fiber-reinforced polypropylene high-impact electric vehicle covering proprietary material and its application |
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