CN109679203A - A kind of Halogen glass fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
A kind of Halogen glass fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08K3/32—Phosphorus-containing compounds
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- 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
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- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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Abstract
The present invention discloses a kind of Halogen glass fiber reinforced polypropylene composite material and preparation method thereof, the preparation of the material is the hydrogen bond action between glass fibre and carbon forming agent using coupling agent treatment, carbon forming agent is adsorbed in fiberglass surfacing, obtains the modified glass fiber reinforcements in surface；After the method that acrylic resin, the glass fiber reinforcements of modification, expansion type flame retardant, compatilizer and antioxidant are passed through melt blending is compound, PP composite material is prepared.Since fiberglass surfacing is coated with carbon forming agent, expansion type flame retardant in carbon forming agent and matrix on interface generates synergistic effect, in combustion process, polymer melt reduces the wellability of glass fibre, slow down heat disturbance to alleviate the decomposition and burning of polymer, therefore " wick effect " is effectively canceled.PP composite material flame retardant property of the present invention is good, flame retarding efficiency is high, and mechanical performance is excellent.
Description
Technical field
The invention belongs to field of compound material, are related to a kind of system of halogen-free flameproof glass fiber reinforced polypropylene composite material
Preparation Method prepares a kind of glass fiber reinforcements and anti-flammability for loading carbon forming agent more particularly, to by hydrogen bond action
The PP composite material that energy is good, flame retarding efficiency is high, mechanical performance is excellent.
Background technique
Polypropylene has many advantages, such as good mechanical property, easily molded processing and low cost, be four big versatile materials it
One.In practical engineering applications, in order to make mechanical property reach engine request, it will usually glass fibers be added in polypropylene matrix
Dimension carries out enhancing processing, obtains glass fiber reinforced polypropylene composite material.
Polyacrylic component only has C and H, and oxygen index (OI) only has 17.5 or so, easily burns, and it is hidden to there is very big fire
Suffer from, it is therefore, flame-retardant modified to be carried out to it often through fire retardant is added in polypropylene matrix.Resistance for polypropylene fire retardant
Combustion agent can substantially be divided into three classes: inorganic fire retardants, halogenated flame retardant and expansion type flame retardant.Expansion type flame retardant be it is a kind of with
Nitrogen, phosphorus are the composite flame-retardant agent mainly formed, it is halogen-free, and also do not use antimony oxide as synergist, which exists
Foaming and intumescing when heated, therefore referred to as expansion type flame retardant, it is the environment friendly flame retardant of a kind of high-efficiency low-toxicity.It is advantageous that nothing
Malicious, low cigarette is optimal environmentally friendly fire retardant, also complies with instantly environmentally friendly development trend.
Glass fibre effectively improves polyacrylic mechanical property as enhancing physical efficiency, although glass fibre itself can not
Combustion, but " wick effect " of glass fiber reinforced polypropylene composite material in combustion aggravates its combustion process more
It is strong, therefore, glass fiber reinforced polypropylene composite material it is fire-retardant fire-retardant more difficult than polyacrylic.
Patent CN104693604A reports a kind of halogen-free flame-retardant glass fiber reinforced polypropylene composite material and preparation method thereof,
Wherein used main flame retardant is phosphorus-nitrogen containing flame retardant, and secondary fire retardant is phosphoric acid salt fire retardant, and fire retardant is at high cost, and
The introducing of fire-retardant particles in the base can destroy interface cohesion, so that mechanical property receives large effect.Liu L etc.
(2015 " Composites Science and Technology " volume 121: 9~15) in paper " Interfacial
charring method to overcome the wicking action in glass fiber-reinforced
Polypropylene composite " in propose the fire-retardant mechanism in interface, be grafted a kind of phosphorous resistance in fiberglass surfacing
Agent small molecule DOPO is fired, modified glass fibre, which is added in polypropylene matrix, to be effectively overcomed in combustion process
" wick effect ", but the fire-retardant mechanism in interface is far from making PP composite material reach the flame retardant rating that can be used.Patent
CN200610023796.8 reports swell type combustion-proof glass fiber reinforced polypropylene composite material and preparation method thereof, directly exists
Traditional expansion type flame retardant is added in polypropylene matrix: ammonium polyphosphate, melamine and pentaerythrite will reach preferable resistance
The additive amount of fuel efficiency fruit, fire retardant is very big, this is a kind of test for polyacrylic processing technology and mechanical property.
Summary of the invention
That the purpose of the present invention is to provide a kind of flame retardant properties is good, flame retarding efficiency is high, the excellent halogen-free flameproof of mechanical performance
Glass fiber reinforced polypropylene composite material and preparation method thereof.
The specific technical solution of the present invention is: a kind of Halogen glass fiber reinforced polypropylene composite material, is with coupling agent
Hydrogen bond action between the glass fibre and carbon forming agent of processing adsorbs carbon forming agent in fiberglass surfacing, obtains what surface was modified
Glass fiber reinforcements；By acrylic resin, the glass fiber reinforcements of modification, expansion type flame retardant, compatilizer and antioxygen
Agent by the method for melt blending it is compound after, PP composite material is prepared.
Since fiberglass surfacing is coated with carbon forming agent, the expansion type flame retardant in the carbon forming agent and matrix on interface is generated
It acts synergistically, in combustion process, polymer melt reduces the wellability of glass fibre, slows down heat disturbance to alleviate polymerization
The decomposition and burning of object, therefore " wick effect " is effectively canceled.
The present invention also provides a kind of preparation methods of halogen-free flameproof glass fibre reinforced composites, including walk as follows
It is rapid:
(1) the commercialization glass fibre for weighing 20~40 parts by weight, by it is glass fiber impregnated molar concentration be 0.5~
In the nitric acid solution of 1.5mol/L, dip time is 4~6 hours, is cleaned repeatedly with deionized water to remove in glass fibers dimension table
The sizing agent in face.
(2) in the glass fiber impregnated silane coupling agent after 1~3wt% hydrolysis for obtaining step (1), processing 1~2
Hour, it is cleaned repeatedly with deionized water.
(3) step (2) is obtained it is glass fiber impregnated in the carbon forming agent of 3~5wt%, handle 4~6 hours, spend
Ionized water cleans repeatedly, and the glass fiber reinforcements of surface cladding carbon forming agent are obtained after dry.
(4) high mixer is added in 7~10:3~5:2~4 ratio in the acid source of expansion type flame retardant, gas source and carbon source
Middle mixing, obtains expansion type flame retardant.
(5) glass fibre for obtaining acrylic resin, expansion type flame retardant, compatilizer, antioxidant and step (3) melts
It is blended, through double screw extruder extruding pelletization, obtains the halogen-free flameproof glass fiber reinforced polypropylene composite material.
Wherein, acrylic resin, expansion type flame retardant, compatilizer, antioxidant are added by main feeding, and glass fibre is by double spiral shells
The glass feed hole of bar extruder is sent into, and the double screw extruder is divided into five temperature control sections from feed opening to head, is processed
Process conditions are as follows:
One Qu Wendu: 180~200 DEG C, two area's temperature: 200~220 DEG C, three Qu Wendu: 200~220 DEG C, four Qu Wendu:
180~200 DEG C, five Qu Wendu: 180~200 DEG C.Head temperature: 180~200 DEG C；Screw speed: 150~180r/min.
Contain in the halogen-free flameproof glass fiber reinforced polypropylene composite material: (a) 40~60 parts by weight of polypropylene tree
Rouge, (b) 20~40 parts by weight expansion type flame retardant, (c) glass fibre of 20~40 parts by weight cladding carbon forming agent, (d) 2~6 weight
Measure part compatilizer, (e) 0.4~0.6 parts by weight antioxidant.
The acrylic resin refers to that melt flow rate is the acrylic resin of 2~4g/10min.
The glass fibre is alkali-free high-strength glass fibre, coats the carbon forming agent by hydrogen bond action.
The compatilizer is polypropylene grafted maleic anhydride.
The coupling agent is (3- aminopropyl) triethoxysilane.
The antioxidant is the combination of one or more of irgasfos 168, antioxidant 1010 and antioxidant 628.
Acid source in the expanding fire retardant is any one of ammonium phosphate, ammonium polyphosphate, melamine phosphate.
Gas source in the expanding fire retardant is any one of melamine, melamine cyanurate, polyamide.
Charcoal source in the expanding fire retardant is pentaerythrite, dipentaerythritol, tripentaerythritol, pentaerythritol phosphate
Any one of.
The carbon forming agent be pentaerythrite, dipentaerythritol, tripentaerythritol, pentaerythritol phosphate it is any.
The hydrogen bond that surface is modified, between recycling coupling agent and carbon forming agent is carried out to glass fibre with coupling agent in the present invention
Effect, is prepared the glass fiber reinforcements of load carbon forming agent, and interface phase resistance combustion engine system cooperates with work with matrix phase resistance combustion engine system
With the flame retardant property of polymer not only can be improved but also improved the interface cohesion between reinforcement and matrix, so that mechanical property
Also further raising has been obtained.
Detailed description of the invention
Fig. 1 is that layer of charcoal of the glass fiber reinforced polypropylene composite material of comparative example 1 after taper calorimetric test scans electricity
Mirror figure；
Fig. 2 is that layer of charcoal of the glass fiber reinforced polypropylene composite material of comparative example 2 after taper calorimetric test scans electricity
Mirror figure；
Fig. 3 is 1mol/L nitric acid treatment 5 hours, handles 1 in (3- aminopropyl) triethoxysilane after 3wt% hydrolysis
Hour, the scanning electron microscope (SEM) photograph for the glass fiber reinforcements that the carbon forming agent of 3~5wt% obtains after handling 4 hours；
Fig. 4 is layer of charcoal scanning electron microscope (SEM) photograph of the above-mentioned glass fiber reinforced polypropylene composite material after taper calorimetric test.
Specific embodiment
In order to deepen the understanding of the present invention, following embodiment is proposed, but protection scope of the present invention is not limited in reality
Apply example.Other variations for made without departing substantially from spirit of that invention and protection scope to those skilled in the art and
Modification is still comprising within that scope of the present invention.
Comparative example 1
By the untreated glass fibre of 20 parts by weight, 3 parts by weight of compatible agent, 0.5 parts by weight irgasfos 168 and 76.5
The polypropylene of part is compound by extrusion molding process, obtains the PP composite material in this example.
Fig. 1 is that layer of charcoal of the glass fiber reinforced polypropylene composite material of comparative example 1 after taper calorimetric test scans electricity
Mirror figure.
Comparative example 2
Ammonium polyphosphate, melamine cyanurate and dipentaerythritol are mixed in the ratio of 8:4:3, obtain expansion type flame-retarding
Agent；By the untreated glass fibre of 20 parts by weight, 30 parts by weight expansion type flame retardants, 3 parts by weight of compatible agent, 0.5 parts by weight
Irgasfos 168 is compound by extrusion molding process with 46.5 parts of polypropylene, obtains the glass fiber reinforced polypropylene in this example
Composite material.
Fig. 2 is that layer of charcoal of the glass fiber reinforced polypropylene composite material of comparative example 2 after taper calorimetric test scans electricity
Mirror figure.
Embodiment 1
The commercialization glass fibre for weighing 20 parts by weight impregnates glass fibre 5 hours in the nitric acid solution of 1mol/L,
It in (3- aminopropyl) triethoxysilane after 3wt% hydrolysis, handles 1 hour, in the carbon forming agent of 5wt%, processing 4 is small
When, obtain the glass fiber reinforcements of surface cladding carbon forming agent；Ammonium polyphosphate, melamine cyanurate and dipentaerythritol are pressed
The ratio of 8:4:3 mixes, and obtains expansion type flame retardant；By above-mentioned 20 parts by weight of glass fiber, 30 parts by weight expansion type flame retardants,
3 parts by weight of compatible agent, the irgasfos 168 of 0.5 parts by weight are compound by extrusion molding process with 46.5 parts of polypropylene, obtain this
Glass fiber reinforced polypropylene composite material in example.
Fig. 3 is 1mol/L nitric acid treatment 5 hours, handles 1 in (3- aminopropyl) triethoxysilane after 3wt% hydrolysis
Hour, the scanning electron microscope (SEM) photograph for the glass fiber reinforcements that the carbon forming agent of 3~5wt% obtains after handling 4 hours；
Fig. 4 is layer of charcoal scanning electron microscope (SEM) photograph of the above-mentioned glass fiber reinforced polypropylene composite material after taper calorimetric test.
Embodiment 2
The commercialization glass fibre for weighing 20 parts by weight impregnates glass fibre 5 hours in the nitric acid solution of 1mol/L,
It in the silane coupling agent after 3wt% hydrolysis, handles 1 hour, in the carbon forming agent of 5wt%, handles 5 hours, obtain surface packet
Cover the glass fiber reinforcements of carbon forming agent；Ammonium polyphosphate, melamine cyanurate and dipentaerythritol are mixed in the ratio of 7:4:3
It closes, obtains expansion type flame retardant；By above-mentioned 20 parts by weight of glass fiber, 30 parts by weight expansion type flame retardants, 3 parts by weight of compatible
Agent, the irgasfos 168 of 0.5 parts by weight are compound by extrusion molding process with 46.5 parts of polypropylene, obtain poly- third in this example
Alkene composite material.
Embodiment 3
The commercialization glass fibre for weighing 20 parts by weight impregnates glass fibre 5 hours in the nitric acid solution of 1mol/L,
It in the silane coupling agent after 3wt% hydrolysis, handles 1 hour, in the carbon forming agent of 3wt%, handles 4 hours, obtain surface packet
Cover the glass fiber reinforcements of carbon forming agent；Ammonium polyphosphate, melamine cyanurate and dipentaerythritol are mixed in the ratio of 8:4:3
It closes, obtains expansion type flame retardant；By above-mentioned 20 parts by weight of glass fiber, 28 parts by weight expansion type flame retardants, 3 parts by weight of compatible
Agent, the irgasfos 168 of 0.5 parts by weight are compound by extrusion molding process with 46.5 parts of polypropylene, obtain poly- third in this example
Alkene composite material.
The glass fiber reinforced polypropylene composite material prepared in comparative example 1~2 and Examples 1 to 3 is containing 20%
Glass fibre.To the batten of comparative example 1~2 and Examples 1 to 3 carry out mechanical property, horizontal vertical burning, oxygen index (OI) test with
And taper calorimetric test, test result are shown in Table 1.
From the test result to comparative example 1~2 and Examples 1 to 3 it is found that LOI, UL-94 combustion rating of each embodiment
And the related data of taper calorimetric test is superior to comparative example, it was demonstrated that can improve polypropylene after glass fiber loaded carbon forming agent
" wick effect " generated in combustion process mentions to reach the synergistic effect of the fire-retardant mechanism in interface Yu matrix phase resistance combustion engine
The flame retardant property of high PP composite material.
The mechanical property and flame retardant property of 1 20% glass fiber reinforced polypropylene composite material of table
Claims (10)
1. a kind of Halogen glass fiber reinforced polypropylene composite material, which is characterized in that be the glass fibre with coupling agent treatment
Hydrogen bond action between carbon forming agent adsorbs carbon forming agent in fiberglass surfacing, obtains the modified glass fiber reinforcements in surface；
Acrylic resin, the glass fiber reinforcements of modification, expansion type flame retardant, compatilizer and antioxidant are passed through into melt blending
After method is compound, PP composite material is prepared.
2. a kind of preparation method of halogen-free flameproof glass fiber reinforced polypropylene composite material, which is characterized in that including walking as follows
It is rapid:
(1) the commercialization glass fibre for weighing 20~40 parts by weight, by it is glass fiber impregnated molar concentration be 0.5~
In the nitric acid solution of 1.5mol/L, dip time is 4~6 hours, is cleaned repeatedly with deionized water to remove in glass fibers dimension table
The sizing agent in face.
(2) it in the glass fiber impregnated silane coupling agent after 1~3wt% hydrolysis for obtaining step (1), handles 1-2 hours,
It is cleaned repeatedly with deionized water.
(3) step (2) is obtained it is glass fiber impregnated in the carbon forming agent of 3~5wt%, handle 4~6 hours, use deionization
Water cleans repeatedly, and the glass fiber reinforcements of surface cladding carbon forming agent are obtained after dry.
(4) acid source of expansion type flame retardant, gas source and carbon source are added in high mixer and are mixed in 7~10:3~5:2~4 ratio
It is even, obtain expansion type flame retardant.
(5) glass fibre for obtaining acrylic resin, expansion type flame retardant, compatilizer, antioxidant and step (3) melts altogether
It is mixed, through double screw extruder extruding pelletization, obtain the halogen-free flameproof glass fiber reinforced polypropylene composite material；
Wherein, acrylic resin, expansion type flame retardant, compatilizer, antioxidant are added by main feeding, and glass fibre is squeezed by twin-screw
The glass feed hole of machine is sent into out, and the double screw extruder is divided into five temperature control sections, processing technology from feed opening to head
Condition are as follows:
One Qu Wendu: 180~200 DEG C, two area's temperature: 200~220 DEG C, three Qu Wendu: 200~220 DEG C, four Qu Wendu: 180
~200 DEG C, five Qu Wendu: 180~200 DEG C.Head temperature: 180~200 DEG C；Screw speed: 150~180r/min.
Contain in the halogen-free flameproof glass fiber reinforced polypropylene composite material: (a) 40~60 parts by weight of polypropylene resin,
(b) 20~40 parts by weight expansion type flame retardant, (c) glass fibre of 20~40 parts by weight cladding carbon forming agent, (d) 2~6 parts by weight
Compatilizer, (e) 0.4~0.6 parts by weight antioxidant.
3. preparation method according to claim 2, which is characterized in that the acrylic resin refers to that melt flow rate is
The acrylic resin of 2~4g/10min.
4. preparation method according to claim 2, which is characterized in that the glass fibre is alkali-free high-strength glass fibre,
The carbon forming agent is coated by hydrogen bond action.
5. preparation method according to claim 2, which is characterized in that the compatilizer is polypropylene grafted maleic anhydride.
6. preparation method according to claim 2, which is characterized in that the coupling agent is (3- aminopropyl) triethoxy
Silane.
7. preparation method according to claim 2, which is characterized in that the antioxidant is irgasfos 168, antioxidant 1010
With the combination of one or more of antioxidant 628.
8. preparation method according to claim 2, which is characterized in that acid source in the expanding fire retardant be ammonium phosphate,
Any one of ammonium polyphosphate, melamine phosphate.
9. preparation method according to claim 2, which is characterized in that the gas source in the expanding fire retardant is melamine
Any one of amine, melamine cyanurate, polyamide.
10. preparation method according to claim 2, which is characterized in that charcoal source and carbon forming agent in the expanding fire retardant
For any one of pentaerythrite, dipentaerythritol, tripentaerythritol, pentaerythritol phosphate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591567A (en) * | 2022-02-21 | 2022-06-07 | 江苏金发科技新材料有限公司 | Glass fiber reinforced flame-retardant polypropylene composite material and preparation method and application thereof |
| CN115011041A (en) * | 2022-07-15 | 2022-09-06 | 中广核俊尔(浙江)新材料有限公司 | Environment-friendly high-gloss low-floating-fiber continuous reinforced long glass fiber polypropylene composite material |
| CN115246966A (en) * | 2022-07-08 | 2022-10-28 | 湖北合聚新材料有限公司 | Expansion flame-retardant polypropylene composition, polypropylene composite material and preparation method thereof |
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| CN1807497A (en) * | 2006-02-08 | 2006-07-26 | 华东理工大学 | Swell type combustion-proof glass fiber reinforced polypropylene composite material and its preparation method |
| CN101343392A (en) * | 2008-08-27 | 2009-01-14 | 蔡增坤 | Halogen-free flame-proof reinforced polypropylene composite material and preparation thereof |
| CN102372907A (en) * | 2010-08-23 | 2012-03-14 | 上海锦湖日丽塑料有限公司 | Halogen-free flame retarding and glass fiber reinforced resin and its preparation method |
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| CN104693604A (en) * | 2015-03-17 | 2015-06-10 | 苏州安鸿泰新材料有限公司 | Halogen-free flame retardant glass-fiber reinforced polypropylene composite material and preparation method thereof |
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| CN115246966A (en) * | 2022-07-08 | 2022-10-28 | 湖北合聚新材料有限公司 | Expansion flame-retardant polypropylene composition, polypropylene composite material and preparation method thereof |
| CN115011041A (en) * | 2022-07-15 | 2022-09-06 | 中广核俊尔(浙江)新材料有限公司 | Environment-friendly high-gloss low-floating-fiber continuous reinforced long glass fiber polypropylene composite material |
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