CN102850646A - Flame-retardant antistatic high-strength thermoplastic composite material and its preparation method - Google Patents
Flame-retardant antistatic high-strength thermoplastic composite material and its preparation method Download PDFInfo
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Abstract
The invention belongs to polymer modification technical field and processing technology field, and discloses a flame-retardant antistatic high-strength thermoplastic composite material and its preparation method. The material comprises (by weight share) 80-100 thermoplastic resin, 50-120 reinforcing fiber, 8-18 flame retardant, 0-5 flame retardant synergistic agent, 0.5-1.8 antistatic agent, 15-30 compatibilizer, 4-10 composite antioxidants, and 0-80 other additives. The invention also discloses the thermoplastic composite material preparation method. The inventive lame-retardant antistatic high-strength thermoplastic composite material has high tension and bending strength, high impact resistance property at low and high temperature, obvious antistatic property, high flame-retardant and fire proof performance. It can reach UL-94 V-O level standard.
Description
Technical field
The invention belongs to macromolecule modified technical field and processing technique field, relate to a kind of fire retardant, antistatic high-strength thermoplastic matrix material and preparation method thereof.
Background technology
In strengthening the thermoplas tic resin composite, because intensity is high, comprehensive mechanical property good, some aspect is replacing steel, i.e. so-called " to mould Dai Gang ".But in existing enhancing thermoplas tic resin composite, owing to not considering the improvement to resin property, therefore its rigidity, flexural strength, tensile strength, shock strength can't reach requirement fully, also often run into inflammable ignite and the defective of static hazard hinders in using strengthening thermoplastic composite.
Normal during plastics use at present some improves really in the flame retardant resistance aspect by adding some fire retardants, but mostly the fire retardant that adds is Halogen.Chinese patent CN00820086.6 has announced a kind of polypropylene resin composite of halogen containing flame-retardant additive, this material still can keep excellent flame retardant properties after long-time outdoor exposure and hydro-thermal dip treating, even when thin thickness, also shown good flame retardant properties, but the amount of being fuming is large during burning, produce in a large number poisonous, corrosive gases, cause so-called " secondary pollution ", give and put out a fire, escape and resume work and bring very large difficulty.Commonly used also have expansion type flame retardant, and this based flame retardant is a kind of flame-retarded technology that grows up on the basis that is applied to anti-flaming dope take phosphorus, nitrogen as main component.When the superpolymer that contains expansion type flame retardant was heated burning, surface energy generated one deck carbonaceous foam layer, can be heat insulation, oxygen barrier, press down cigarette, and can prevent the molten drop behavior, have good flame retardant properties.Chinese patent CN03138746.2 discloses a kind of non-halogen flameproof polypropylene materials, contains expansion type flame retardant, and result of use is really fine.But, in order to reach certain flame retardant effect, need add-on larger, just general addition can obtained positive effect more than 40%.And this expansion type fire retardant is polar material, and nonpolar resin compatible is poor, and a large amount of these based flame retardants of interpolation will inevitably cause the significant decline of material mechanical performance in resin.
In thermoplas tic resin composite's industrial production, the impact of static is also more and more serious.Static hinders normal complete processing, and is especially outstanding especially in the synthetic fiber industry.Frictional electricity produce to attract or repulsive force, make synthon in spinning, drawing-off, weave cotton cloth, difficulty all occurs in each procedure such as packing.Electrostatic interaction also damages quality product, and for example superpolymer affects the quality of material owing to electrostatic adhesion dust or aqueous vapor.The spark discharge that static causes under the occasion that has flammable and explosive substance to exist, can lead to huge calamity.Someone adds up, and the accident in the chemical industry is nearly 1st/10th, and is caused by static.
Therefore, how in conjunction with prior art, improving fire-retardant, static resistance and the comprehensive mechanical property of thermoplastic resin, develop a kind of fire retardant, antistatic high-strength thermoplastic matrix material, is to make thermoplas tic resin composite's range of application become necessary means wide and that open up markets.
Summary of the invention
The defective that exists in order to overcome above-mentioned prior art, the purpose of this invention is to provide a kind of fire retardant, antistatic high-strength thermoplastic matrix material, this material has high shock resistance under very high stretching and flexural strength and the low and high temperature, static resistance is remarkable, the fire-retardant fireproof performance is high, can reach the V-0 grade standard of UL-94.
Another object of the present invention provides above-mentioned fire retardant, antistatic high-strength thermoplastic composite manufacture method.
Technical scheme of the present invention is as follows:
The invention provides a kind of fire retardant, antistatic high-strength thermoplastic matrix material, this material comprises following component and weight part: 80~100 parts of thermoplastic resins, 50~120 parts of fortifying fibres, 8~18 parts of fire retardants, 0~5 part of fire retarding synergist, 0.5~1.8 part of static inhibitor, 15~30 parts of compatilizers, 4~10 parts of complex type antioxidants and 0~80 part of other auxiliary agent.
Described thermoplastic resin is selected from a kind of in polypropylene, high density polyethylene(HDPE), Low Density Polyethylene, polystyrene, polyphenylene oxide or the polyoxymethylene.
Described fortifying fibre is selected from any one in glass fibre, carbon fiber, polyster fibre, nylon fiber, steel fiber or the metal oxide.
Described fire retardant is selected from trimeric cyanamide, melamine cyanurate, melamine phosphate, melamine polyphosphate, melamine pyrophosphate, trimeric cyanamide octamolybdate, melamine borate salt, coats one or more in polyphosphoric acid amine, magnesium hydroxide, aluminium hydroxide, decabromodiphenyl oxide, tetrabromo-bisphenol, chlorinatedpolyethylene or the clorafin; Wherein: coated ammonium polyphosphate is selected from one or more in melamine-formaldehyde coated ammonium polyphosphate, Resins, epoxy coated ammonium polyphosphate, unsaturated polyester coated ammonium polyphosphate, EVA coated ammonium polyphosphate or the polyurethane elastomer coated ammonium polyphosphate.
Described fire retarding synergist is selected from one or more in calcium oxide, aluminum oxide, boron trioxide, titanium oxide, zinc oxide, magnesium oxide, silicon oxide, zinc borate, hydrotalcite or the antimonous oxide.
Described static inhibitor is selected from a kind of in conductive acetylene carbon black, ethylene glycol lauric amide, sodium sulfonate, octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate (static inhibitor SN) or two (beta-hydroxyethyl) stearylamine (antistatic agent B 2).
Described compatilizer is selected from a kind of in maleic anhydride inoculated polypropylene, acrylic acid-grafted polypropylene, maleic anhydride grafted polyethylene, acrylic acid-grafted polyethylene, maleic anhydride graft EPDM or the acrylic acid-grafted ethylene-octene copolymer.
Described complex type antioxidant is selected from N, N '-two (betanaphthyl) Ursol D, thio-2 acid octadecyl ester, [β-(3,5 di-t-butyl 4-hydroxyl-phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), Tyox B (anti-oxidant DLTP) or 1, the mixture of one or more in 1,3-three (2-methyl-4-hydroxyl-5-trimethylphenylmethane base) butane (antioxidant CA).
Described other auxiliary agent is selected from one or more in kaolin, talcum powder, calcium carbonate or the glass microballon.
The present invention also provides a kind of above-mentioned fire retardant, antistatic high-strength thermoplastic composite manufacture method, and the method may further comprise the steps:
(1) with 0~80 part of 80~100 parts of thermoplastic resins, 8~18 parts of fire retardants, 0~5 part of fire retarding synergist, 0.5~1.8 part in static inhibitor, 15~30 parts of compatilizers, 4~10 parts of complex type antioxidants and other auxiliary agent, put into high-speed mixer, pre-mixing 8~15min, temperature is 80~100 ℃;
(2) more mixed material is placed the high pressure static electricity fluidized-bed, 50~120 parts of fortifying fibres are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of fortifying fibre polymeric adsorbent, make the parts by weight of thermoplastic resin remain on 80~100 parts;
(3) absorption has the fortifying fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet.
Described high-speed mixer rotating speed is 600~2000r/min, and rotating speed is preferably 1000~1600r/min.
Described die temperature is 160~250 ℃, and pressure is 8~16MPa; Temperature is preferably 180~200 ℃, and pressure is preferably 12~15MPa.
The present invention compares with prior art, has following advantage and beneficial effect:
1, compared with prior art, fire retardant, antistatic high-strength thermoplastic matrix material of the present invention has high shock resistance under very high stretching and flexural strength and the low and high temperature, satisfies the deficiency of composite materials property.
2, thermoplastic composite static resistance of the present invention is remarkable, greatly reduces the harm that static brings in the industrial production; The fire-retardant fireproof performance also reaches the V-0 grade standard of UL-94, makes the application of product more extensive.
3, thermoplastic composite of the present invention is widely used in the plastics such as household electric appliances, chemical building material.According to the relevent statistics, the fire retardant, antistatic of product will make range of product satisfy rate and domestic market occupation rate all above 95%.The fire retardant, antistatic high-strength thermoplastic matrix material of this optimization modification makes goods more superior, applicable, this shows that the matrix material of modification will bring the great market space to China's material market.
4, thermoplastic composite of the present invention has been filled up the blank of fire retardant, antistatic high-strength thermoplastic matrix material, is widely used in the plastics such as industrial building materials, automotive trim.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Adopt GB (GB) to measure the properties of material among the embodiment, if no special instructions, the umber of component is parts by weight.
Embodiment 1
First 18 parts of 30 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 100 parts of polypropylene powder resins, 5 parts of Resins, epoxy coated ammonium polyphosphates and 4 parts of melamine cyanurates, 2 parts of antimonous oxides, 0.5 part of two (beta-hydroxyethyl) stearylamine, 2 parts of anti-oxidant DLTPs and 4 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 10min with 1200r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 55 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 100 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 180 ℃, 12MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 2
First 15 parts of complex type antioxidant, the maleic anhydride inoculated polypropylenes of 90 parts of polypropylene powder resins, 7 parts of Resins, epoxy coated ammonium polyphosphates and 5 parts of melamine cyanurates, 3 parts of antimonous oxides, 0.8 part of two (beta-hydroxyethyl) stearylamine, 3 parts of anti-oxidant DLTPs and 5 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 8min with 1400r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 75 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 100 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 190 ℃, 13MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 3
First 20 parts of 50 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 100 parts of polypropylene powder resins, 8 parts of Resins, epoxy coated ammonium polyphosphates and 6 parts of melamine cyanurates, 1.2 parts of two (beta-hydroxyethyl) stearylamines, 3 parts of anti-oxidant DLTPs and 2 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 12min with 1500r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 100 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 100 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 200 ℃, 15MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 4
First 24 parts of 60 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 100 parts of polypropylene powder resins, 10 parts of Resins, epoxy coated ammonium polyphosphates and 8 parts of melamine cyanurates, 5 parts of antimonous oxides, 1.4 parts of two (beta-hydroxyethyl) stearylamines, 4 parts of anti-oxidant DLTPs and 4 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 15min with 1000r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 120 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 100 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 195 ℃, 13MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 5
First 28 parts of 80 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 80 parts of polypropylene powder resins, 8 parts of Resins, epoxy coated ammonium polyphosphates and 8 parts of melamine cyanurates, 4 parts of antimonous oxides, 1.8 parts of two (beta-hydroxyethyl) stearylamines, 5 parts of anti-oxidant DLTPs and 5 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 12min with 1200r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 120 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 80 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 190 ℃, 14MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 1
Do not add fire retardant (Resins, epoxy coated ammonium polyphosphate, melamine cyanurate, antimonous oxide) in the compound, all the other are with embodiment 4.First 24 parts of 60 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 100 parts of polypropylene powder resins, 1.4 parts of two (beta-hydroxyethyl) stearylamines, 4 parts of anti-oxidant DLTPs and 4 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 15min with 1000r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 120 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 100 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 195 ℃, 13MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 2
Do not add static inhibitor (two (beta-hydroxyethyl) stearylamine) in the compound, all the other are with embodiment 5.First 28 parts of 80 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 80 parts of polypropylene powder resins, 8 parts of Resins, epoxy coated ammonium polyphosphates and 8 parts of melamine cyanurates, 4 parts of antimonous oxides, 5 parts of anti-oxidant DLTPs and 5 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 12min with 1200r/min, temperature is at 80~100 ℃; Again mixed material is placed the high pressure static electricity fluidized-bed, 120 parts of glass fibre are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of glass fibre polymeric adsorbent, make the parts by weight of acrylic resin remain on 80 parts; Absorption has the glass fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet under 190 ℃, 14MPa pressure; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 3
Do not add fortifying fibre (glass fibre) in the compound, all the other are with embodiment 5.First 28 parts of 80 parts of complex type antioxidant, talcum powder, the maleic anhydride inoculated polypropylenes of 80 parts of polypropylene powder resins, 8 parts of Resins, epoxy coated ammonium polyphosphates and 8 parts of melamine cyanurates, 4 parts of antimonous oxides, 1.8 parts of two (beta-hydroxyethyl) stearylamines, 5 parts of anti-oxidant DLTPs and 5 parts of compositions of antioxidant 1010 are assorted raw material by weight, then place the high-speed mixer pre-mixing 12min with 1200r/min, temperature is at 80~100 ℃; Then pass through from baking oven and high temperature die head, pass through again mould, under 190 ℃, 14MPa pressure, make composite sheet; Sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Table 1
Found out by every data in the table 1, the over-all properties of embodiment 4,5 gained matrix materials is better, can improve the plastic prod performance.Do not add fire retardant in the comparative example 1 the matrix material oxygen index is significantly reduced, flame retardant resistance does not reach the product performance requirement; Comparative example 2 does not add static inhibitor makes matrix material volume resistivity very large, and static resistance is very poor; It is very poor that comparative example 3 does not add the mechanical property (tensile strength, tensile modulus, flexural strength, notched Izod impact strength) that fortifying fibre makes matrix material, and comprehensive mechanical property does not far reach the product performance requirement.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. thermoplastic composite, it is characterized in that: this material comprises following component and weight part: 80~100 parts of thermoplastic resins, 50~120 parts of fortifying fibres, 8~18 parts of fire retardants, 0~5 part of fire retarding synergist, 0.5~1.8 part of static inhibitor, 15~30 parts of compatilizers, 4~10 parts of complex type antioxidants and 0~80 part of other auxiliary agent.
2. thermoplastic composite according to claim 1 is characterized in that: described thermoplastic resin is selected from a kind of in polypropylene, high density polyethylene(HDPE), Low Density Polyethylene, polystyrene, polyphenylene oxide or the polyoxymethylene; Described fortifying fibre is selected from any one in glass fibre, carbon fiber, polyster fibre, nylon fiber, steel fiber or the metal oxide.
3. thermoplastic composite according to claim 1 is characterized in that: described fire retardant is selected from trimeric cyanamide, melamine cyanurate, melamine phosphate, melamine polyphosphate, melamine pyrophosphate, trimeric cyanamide octamolybdate, melamine borate salt, coats one or more in polyphosphoric acid amine, magnesium hydroxide, aluminium hydroxide, decabromodiphenyl oxide, tetrabromo-bisphenol, chlorinatedpolyethylene or the clorafin; Wherein: coated ammonium polyphosphate is selected from one or more in melamine-formaldehyde coated ammonium polyphosphate, Resins, epoxy coated ammonium polyphosphate, unsaturated polyester coated ammonium polyphosphate, EVA coated ammonium polyphosphate or the polyurethane elastomer coated ammonium polyphosphate.
4. thermoplastic composite according to claim 1, it is characterized in that: described fire retarding synergist is selected from one or more in calcium oxide, aluminum oxide, boron trioxide, titanium oxide, zinc oxide, magnesium oxide, silicon oxide, zinc borate, hydrotalcite or the antimonous oxide.
5. thermoplastic composite according to claim 1 is characterized in that: described static inhibitor is selected from a kind of in conductive acetylene carbon black, ethylene glycol lauric amide, sodium sulfonate, octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate or two (beta-hydroxyethyl) stearylamine.
6. thermoplastic composite according to claim 1 is characterized in that: described compatilizer is selected from a kind of in maleic anhydride inoculated polypropylene, acrylic acid-grafted polypropylene, maleic anhydride grafted polyethylene, acrylic acid-grafted polyethylene, maleic anhydride graft EPDM or the acrylic acid-grafted ethylene-octene copolymer.
7. thermoplastic composite according to claim 1, it is characterized in that: described complex type antioxidant is selected from N, N '-two (betanaphthyl) Ursol D, thio-2 acid octadecyl ester, [β-(3,5 di-t-butyl 4-hydroxyl-phenyl) propionic acid] pentaerythritol ester, Tyox B or 1, the mixture of one or more in 1,3-three (2-methyl-4-hydroxyl-5-trimethylphenylmethane base) butane.
8. thermoplastic composite according to claim 1, it is characterized in that: described other auxiliary agent is selected from one or more in kaolin, talcum powder, calcium carbonate or the glass microballon.
9. the preparation method of the arbitrary described thermoplastic composite of claim 1 to 8, it is characterized in that: the method may further comprise the steps:
(1) with 0~80 part of 80~100 parts of thermoplastic resins, 8~18 parts of fire retardants, 0~5 part of fire retarding synergist, 0.5~1.8 part in static inhibitor, 15~30 parts of compatilizers, 4~10 parts of complex type antioxidants and other auxiliary agent, put into high-speed mixer, pre-mixing 8~15min, temperature is 80~100 ℃;
(2) more mixed material is placed the high pressure static electricity fluidized-bed, 50~120 parts of fortifying fibres are passed through from fluidized-bed continuously, regulate the electrostatic potential of fluidized-bed to regulate the amount of fortifying fibre polymeric adsorbent, make the parts by weight of thermoplastic resin remain on 80~100 parts;
(3) absorption has the fortifying fibre of resin to pass through from baking oven and high temperature die head continuously, passes through mould again, makes composite sheet.
10. the preparation method of thermoplastic composite according to claim 9, it is characterized in that: described high-speed mixer rotating speed is 600~2000r/min, and rotating speed is preferably 1000~1600r/min; Described die temperature is 160~250 ℃, and pressure is 8~16MPa; Temperature is preferably 180~200 ℃, and pressure is preferably 12~15MPa.
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