CN105061896A - Halogen-free flame-retardant LGFPP (long glass fiber reinforced polypropylene) material and preparation method thereof - Google Patents
Halogen-free flame-retardant LGFPP (long glass fiber reinforced polypropylene) material and preparation method thereof Download PDFInfo
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- CN105061896A CN105061896A CN201510512088.XA CN201510512088A CN105061896A CN 105061896 A CN105061896 A CN 105061896A CN 201510512088 A CN201510512088 A CN 201510512088A CN 105061896 A CN105061896 A CN 105061896A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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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
- C08L2201/22—Halogen free composition
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Abstract
The invention discloses a halogen-free flame-retardant LGFPP (long glass fiber reinforced polypropylene) material which comprises the following raw material components: 45-75 parts of polypropylene, 15-40 parts of long glass fiber, 6-13 parts of a compatilizer, 0.6-1.4 parts of an anti-oxidant, 8-25 parts of an intumescent flame retardant and 2-15 parts of a synergistic agent. During the preparation of the material, the dried polypropylene and compatilizer are uniformly mixed with the anti-oxidant to be subjected to blending extrusion; a melt dips fiberglass through a dipping runner; the polypropylene, intumescent flame retardant, sepiolite subjected to acidizing treatment and compatilizer are taken and subjected to drying treatment; the dried raw materials are mixed with the anti-oxidant to be subjected to blending extrusion; the dipped fiberglass material bars are coated with the mixed raw materials extruded, and cooling and granulating are carried out, so that the halogen-free flame-retardant long glass fiber reinforced polypropylene composite material is obtained. According to the invention, the technical problems that the LGFPP material in the prior art can discharge poisonous and corrosive gas and the like during combustion, and the mechanical property and cost performance are relatively low are solved.
Description
Technical field
The invention belongs to long glass fiber-reinforced polypropylene materials and preparing technical field, particularly relate to a kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials and preparation method thereof.
Background technology
Long glass fiber-reinforced polypropylene LGFPP has following remarkable advantage: good shock strength, flexural strength, tensile strength, high temperature resistant, good stability of the dimension, excellent fatigue performance etc., obtain widespread use at industrial circles such as automobile, electrical equipment, aviations.But there is " wick effect " in LGFPP, limiting oxygen index(LOI) value is very low; Be the incendive material of a kind of appearance, and combustion processes thermal value is large.The requirement do not reached in some field of LGFPP flame retardant properties, therefore needs to carry out flame-retardant modified to it.What the industrial fire retardant for the flame-retardant modified interpolation of LGFPP was more at present is halogen flame, although the flame retardant effect of halogen flame is very good, from environmental angle, can release poisonous and corrosive gases etc., can cause secondary pollution during its burning.Therefore, develop a suitable halogen-free flame-retardant glass fiber reinforced polypropylene system, obtaining the halogen-free flame-retardant glass fiber reinforced polypropylene technology having excellent flame retardant performance, higher force performance and cost performance high is highly significant.
Summary of the invention
The technical problem to be solved in the present invention: a kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials and preparation method thereof is provided, poisonous and corrosive gases etc. can be released during the burning adopting halogen flame to exist with the LGFPP material solving prior art, secondary pollution can be caused, mechanical property and the technical problem such as cost performance is low.
Technical solution of the present invention:
A kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials, by mass parts, this material feedstock composition comprises: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part, described roving glass fiber is the continuous glass fibre of diameter 5-20 micron, compatilizer maleic anhydride graft PP compatilizer, oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
Described expansion type flame retardant is take tetramethylolmethane as the young laying ducks in cage of base or the mixture of tetramethylolmethane and melamine polyphosphate or trimeric cyanamide.
Described take tetramethylolmethane as the young laying ducks in cage of base or tetramethylolmethane content is 6-18 part; Melamine polyphosphate or content of melamine are 2-15 part.
Described synergist is in block, earthy or the sepiolite of fibrous agrregate, and the crystal water of sepiolite, planar water and water of constitution total content, at 5-18%, adopt concentration to be that 0.1-3.2mol/L hydrochloric acid carries out acidification.
The preparation method of described halogen-free flameproof long glass fiber-reinforced polypropylene materials, it comprises:
Step 1, according to material composition mass parts ratio: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part get out various raw material;
Step 2, get 35-50 part polypropylene and 2-7 part compatilizer by drying treatment, drying temperature 70-90 DEG C, time of drying 6-10h;
Step 3, dried polypropylene and compatilizer are mixed with 0.2-0.5 part oxidation inhibitor after put in twin screw extruder and carry out blending extrusion, twin screw extruder temperature is set as 160-215 DEG C;
Step 4, the melt after extruding to be flooded 15-40 part glass fibre by dipping runner, obtain glass fiber impregnated material strip;
Step 5, get the sepiolite after 10-40 part polypropylene, 8-25 part expansion type flame retardant and 2-15 part acidification and 4-11 part compatilizer through drying treatment;
Step 6, each raw material dried in step 5 to be mixed with 0.4-0.9 part oxidation inhibitor, add after raw material is mixed in forcing machine and carry out blending extrusion;
Step 7, be coated in the glass fiber impregnated material strip described in step 4 by the mixing raw material after extruding, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material.
Beneficial effect of the present invention:
Present invention employs technique scheme, compared with the prior art, the present invention adopts polypropylene as matrix resin, using maleic anhydride graft PP as compatilizer, this compatilizer enhances the interface binding power of glass fibre and acrylic resin, and adopt single stage method to prepare halogen-free flameproof long fibre enhanced polypropylene matrix material, complete the dipping of matrix resin to fiber by continuous print fiber by impregnation mold, finally complete in coating mould with halogen-free flame retardants matrix melt dipping material strip on coated; Add halogen-free flame retardants in fiber glass reinforced polypropylene material and not only obtain good flame retardant effect, effectively slow down " wick effect " of glass, and the problem of environmental pollution avoiding use halogenated flame retardant to bring; Halogen-free flameproof long glass fiber-reinforced polypropylene materials of the present invention has good mechanical property, excellent flame retardancy, and reduction production cost, the competitive power of product gets a promotion, poisonous and corrosive gases etc. can be released during the burning that the LGFPP material solving prior art adopts halogen flame to exist, secondary pollution can be caused, mechanical property and the technical problem such as cost performance is low.
Embodiment
A kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials, by mass parts, this material feedstock composition comprises: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part, described roving glass fiber is the continuous glass fibre of diameter 5-20 micron, compatilizer maleic anhydride graft PP compatilizer.Increase the consistency of PP and glass fibre, the mechanical property of matrix material significantly improved), oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.It has low toxicity, tasteless, excellent consistency; Can delay or stop matrix material to be oxidized or autoxidation process, thus extend the work-ing life of material.
Described polypropylene is melt flow rate (MFR) is 100g/10min at 200 DEG C.Advantage: good fluidity, is easy to forming process.
Described expansion type flame retardant comprises: take tetramethylolmethane as the young laying ducks in cage of base or tetramethylolmethane 6-18 part and melamine polyphosphate or trimeric cyanamide 2-15 part.The present invention adopts tetramethylolmethane to be that the young laying ducks in cage of base contains tetramethylolmethane as skeleton, has excellent one-tenth charcoal; Because melamine polyphosphate and tetramethylolmethane are all contain phosphoric acid ester in the young laying ducks in cage of base, acid source and carbon source decompose the poly-metaphosphoric acid that generates larger concentration and fine and close layer of charcoal covers material surface, play the diffusion hindering thermal conduction between polymkeric substance and thermal source and oxygen; And melamine polyphosphate can decompose release non-combustible gas trimeric cyanamide, effectively dilutes the concentration of surrounding materials oxygen, plays the effect that gas phase is fire-retardant.When the content of melamine polyphosphate is very low, although charcoal amount increases in material, material expansion is made to become charcoal owing to lacking enough sources of the gas and acid source; When the content of melamine polyphosphate is higher, because glass easily destroys the continuity of layer of charcoal, cause the layer of charcoal of formation relatively fragile, when melamine polyphosphate produces more gas, can Char Residues Structure be affected.
Described synergist is in block, earthy or the sepiolite of fibrous agrregate, and the crystal water of sepiolite, planar water and water of constitution total content, at 5-18%, adopt concentration to be that 0.1-3.2mol/L hydrochloric acid carries out acidification.
The present invention selects sepiolite to have as its advantage of synergist: 1, sepiolite has higher length-to-diameter ratio, and specific surface area theoretical value is up to 900m2/g, and Heat stability is good, can be used as the modification that support of the catalyst can be used for polymkeric substance; Some surface propertieies of sepiolite, as surperficial slightly acidic (Si-OH) etc., make itself can catalysis some reaction; 2, crystal water, planar water and water of constitution total content are its important parameters, make sepiolite slough crystal water, planar water and water of constitution in combustion, make it absorb a large amount of heats, play the flame retardant effect of heat absorption cooling; 3, the sepiolite after peracid treatment can reduce the content of impurity in sepiolite, and the part Mg2+ on sepiolite surface is replaced by H+ simultaneously, can increase the Si-OH quantity that sepiolite surface is active.Be simultaneously that Si-OH that pyrophosphate salt that the young laying ducks in cage open loop degraded of base is formed is active with sepiolite surface generates and contains the stable crosslinked layer of charcoal of Si-O-P key with tetramethylolmethane in temperature-rise period, the formation of Si-O-P key can inhibit the thermal destruction of burnt poly-phosphate, more phosphorus is made to participate in esterification, improve the content of layer of charcoal, strengthen the intensity of layer of charcoal, thus improve the stability of foamed char, thus play good flame retardant effect.
The preparation method of described halogen-free flameproof long glass fiber-reinforced polypropylene materials, it comprises:
Step 1, according to material composition mass parts ratio: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part get out various raw material;
Step 2, get 35-50 part polypropylene and 2-7 part compatilizer by drying treatment, drying temperature 70-90 DEG C, time of drying 6-10h;
Step 3, dried polypropylene and compatilizer are mixed with 0.2-0.5 part oxidation inhibitor after put in twin screw extruder and carry out blending extrusion, twin screw extruder temperature is set as 160-215 DEG C;
Step 4, the melt after extruding to be flooded 15-40 part glass fibre by dipping runner, obtain glass fiber impregnated material strip;
Step 5, get the sepiolite after 10-40 part polypropylene, 8-25 part expansion type flame retardant and 2-15 part acidification and 4-11 part compatilizer through drying treatment;
Step 6, each raw material dried in step 5 to be mixed with 0.4-0.9 part oxidation inhibitor, add after raw material is mixed in forcing machine and carry out blending extrusion;
Step 7, be coated in the glass fiber impregnated material strip described in step 4 by the mixing raw material after extruding, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material.
Embodiment 1: the preparation method of halogen-free flameproof long glass fiber-reinforced polypropylene materials, get 35 parts of polypropylene and 4 parts of compatilizer drying for standby respectively, above-mentioned dried polypropylene and compatilizer are mixed with 0.5 part of oxidation inhibitor, then in twin screw extruder, blending extrusion is carried out, processing temperature is 210 DEG C, melt is flooded 15 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 40 parts of polypropylene, 25 parts of expansion type flame retardant tetramethylolmethanes and melamine polyphosphate, 2 portions of synergist and 3 parts of compatilizers again and carry out drying, above-mentioned dried material is mixed with 0.6 part of oxidation inhibitor, finally by mixing of materials evenly after add in forcing machine and carry out blending extrusion, when extruding, the mixture of melting is coated in glass fiber impregnated material strip, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material; Described drying temperature is 80 DEG C, and time of drying is 8h.
Embodiment 2: get 35 parts of polypropylene and 4 parts of compatilizer drying for standby respectively, above-mentioned dried polypropylene and compatilizer are mixed with 0.5 part of oxidation inhibitor, then in twin screw extruder, blending extrusion is carried out, processing temperature is 210 DEG C, melt is flooded 30 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 20 parts of polypropylene again, young laying ducks in cage that 25 parts of expansibility flame-proof agent tetramethylolmethanes are base and melamine polyphosphate, 8 portions of synergist and 9 parts of compatilizers carry out drying, above-mentioned dried material is mixed with 0.3 part of oxidation inhibitor, finally by mixing of materials evenly after add in forcing machine and carry out blending extrusion, when extruding, the mixture of melting is coated in glass fiber impregnated material strip, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material; Described drying temperature is 80 DEG C, and time of drying is 8h.
Embodiments of the invention 3: get 50 parts of polypropylene and 4 parts of compatilizer drying for standby respectively, above-mentioned dried polypropylene and compatilizer are mixed with 0.2 part of oxidation inhibitor, then in twin screw extruder, blending extrusion is carried out, processing temperature is 210 DEG C, melt is flooded 40 parts of fibers by dipping runner, obtains fiber impregnation material strip; Get 20 parts of polypropylene again, young laying ducks in cage that 25 parts of expansibility flame-proof agent tetramethylolmethanes are base and trimeric cyanamide, 4 portions of synergist and 3 parts of compatilizers carry out drying, above-mentioned dried material is mixed with 0.9 part of oxidation inhibitor, finally by mixing of materials evenly after add in forcing machine and carry out blending extrusion, when extruding, the mixture of melting is coated in glass fiber impregnated material strip, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material; Described drying temperature is 80 DEG C, and time of drying is 8h.
Salient features is tested: the sample that above-mentioned 3 embodiments draw is made standard testing batten according to standard, and carry out every test and adopt the sample of prior art to contrast, its performance test results is as shown in table 1.
As can be seen from table 1 indices: adopt the preparation-obtained sample of technical scheme of the present invention, compared with the fire-retardant LGFPP material of routine, its mechanical property improves by a relatively large margin, and flame retardant properties is better.Tetramethylolmethane is the cage structure that the young laying ducks in cage molecule of base has rigidity, integrate carbon source and acid source, and melamine polyphosphate is gas collection source and acid source is integrated, the problem poor relative to consistency between conventional expanded type fire retardant three components, tetramethylolmethane is that the young laying ducks in cage of base and the combination of melamine polyphosphate are improved to the consistency between expansion type flame retardant.And because tetramethylolmethane is base, the hydroxyl of young laying ducks in cage compared with tetramethylolmethane (PER) in molecular structure reduces in a large number, molecular polarity weakens, improve the consistency between fire retardant and LGFPP matrix, and fire retardant is also improved in the dispersiveness of LGFPP, improve the flame retardant effect of flame-retardant system.Add synergist after acidification sepiolite, be that the active Si-OH in pyrophosphate salt and sepiolite surface that the young laying ducks in cage open loop degraded of base is formed generates and contains the stable crosslinked layer of charcoal of Si-O-P key with tetramethylolmethane in temperature-rise period, the formation of Si-O-P key can inhibit the thermal destruction of burnt poly-phosphate, more phosphorus is made to participate in esterification, improve the content of layer of charcoal, strengthen the intensity of layer of charcoal, thus improve the stability of foamed char, thus play better flame retardant effect.
Claims (5)
1. a halogen-free flameproof long glass fiber-reinforced polypropylene materials, it is characterized in that: by mass parts, this material feedstock composition comprises: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part, described roving glass fiber is the continuous glass fibre of diameter 5-20 micron, compatilizer maleic anhydride graft PP compatilizer, oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
2. a kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials according to claim 1, is characterized in that: described expansion type flame retardant is take tetramethylolmethane as the young laying ducks in cage of base or the mixture of tetramethylolmethane and melamine polyphosphate or trimeric cyanamide.
3. a kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials according to claim 2, is characterized in that: by mass parts, and described take tetramethylolmethane as the young laying ducks in cage of base or tetramethylolmethane content is 6-18 part; Melamine polyphosphate or content of melamine are 2-15 part.
4. a kind of halogen-free flameproof long glass fiber-reinforced polypropylene materials according to claim 1, it is characterized in that: described synergist is the sepiolite in bulk, earthy or fibrous agrregate, the crystal water of sepiolite, planar water and water of constitution total content, at 5-18%, adopt concentration to be that 0.1-3.2mol/L hydrochloric acid carries out acidification.
5. the preparation method of halogen-free flameproof long glass fiber-reinforced polypropylene materials as claimed in claim 1, it comprises:
Step 1, according to material composition mass parts ratio: polypropylene 45-75 part, roving glass fiber 15-40 part, compatilizer 6-13 part, oxidation inhibitor 0.6-1.4 part, expansion type flame retardant 8-25 part and synergist 2-15 part get out various raw material;
Step 2, get 35-50 part polypropylene and 2-7 part compatilizer by drying treatment, drying temperature 70-90 DEG C, time of drying 6-10h;
Step 3, dried polypropylene and compatilizer are mixed with 0.2-0.5 part oxidation inhibitor after put in twin screw extruder and carry out blending extrusion, twin screw extruder temperature is set as 160-215 DEG C;
Step 4, the melt after extruding to be flooded 15-40 part glass fibre by dipping runner, obtain glass fiber impregnated material strip;
Step 5, get the sepiolite after 10-40 part polypropylene, 8-25 part expansion type flame retardant and 2-15 part acidification and 4-11 part compatilizer through drying treatment;
Step 6, each raw material dried in step 5 to be mixed with 0.4-0.9 part oxidation inhibitor, add after raw material is mixed in forcing machine and carry out blending extrusion;
Step 7, be coated in the glass fiber impregnated material strip described in step 4 by the mixing raw material after extruding, after cooling, pelletizing becomes the particle of 10 ~ 14mm, obtains halogen-free flameproof long fibre enhanced polypropylene matrix material.
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| CN105482255A (en) * | 2015-12-30 | 2016-04-13 | 上海普利特复合材料股份有限公司 | Environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material and preparation method thereof |
| CN108724853A (en) * | 2018-04-28 | 2018-11-02 | 广东聚石化学股份有限公司 | A kind of preparation method of halogen-free expandable fire retardant fiber glass reinforced polypropylene plank |
| CN108948520A (en) * | 2018-06-15 | 2018-12-07 | 常州大学 | One type zeolitic imidazolate framework material cooperates with expanded flame-retardant polypropylene preparation method |
| CN112321940A (en) * | 2020-09-23 | 2021-02-05 | 句容市百事特复合材料有限公司 | Heat-resistant and aging-resistant long glass fiber reinforced PP material and preparation method thereof |
| CN114181464A (en) * | 2019-03-30 | 2022-03-15 | 裴广华 | High-strength glass fiber composite material |
| CN115160689A (en) * | 2022-06-29 | 2022-10-11 | 国网浙江省电力有限公司湖州供电公司 | Flame-retardant material for lithium ion battery packaging and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105482255A (en) * | 2015-12-30 | 2016-04-13 | 上海普利特复合材料股份有限公司 | Environment-friendly flame-retardant long-glass-fiber-reinforced polypropylene composite material and preparation method thereof |
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| CN108724853B (en) * | 2018-04-28 | 2021-04-06 | 广东聚石化学股份有限公司 | Preparation method of halogen-free intumescent flame-retardant glass fiber reinforced polypropylene plate |
| CN108948520A (en) * | 2018-06-15 | 2018-12-07 | 常州大学 | One type zeolitic imidazolate framework material cooperates with expanded flame-retardant polypropylene preparation method |
| CN108948520B (en) * | 2018-06-15 | 2021-04-27 | 常州大学 | Preparation method of zeolite-like imidazole ester framework material synergistic expansion flame-retardant polypropylene |
| CN114181464A (en) * | 2019-03-30 | 2022-03-15 | 裴广华 | High-strength glass fiber composite material |
| CN112321940A (en) * | 2020-09-23 | 2021-02-05 | 句容市百事特复合材料有限公司 | Heat-resistant and aging-resistant long glass fiber reinforced PP material and preparation method thereof |
| CN115160689A (en) * | 2022-06-29 | 2022-10-11 | 国网浙江省电力有限公司湖州供电公司 | Flame-retardant material for lithium ion battery packaging and preparation method and application thereof |
| CN115160689B (en) * | 2022-06-29 | 2023-09-29 | 国网浙江省电力有限公司湖州供电公司 | Flame retardant material for lithium ion battery packaging and preparation method and application thereof |
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Application publication date: 20151118 |