CN104672612B - Flame retardant polypropylene material and preparation method thereof - Google Patents

Flame retardant polypropylene material and preparation method thereof Download PDF

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Publication number
CN104672612B
CN104672612B CN201510056293.XA CN201510056293A CN104672612B CN 104672612 B CN104672612 B CN 104672612B CN 201510056293 A CN201510056293 A CN 201510056293A CN 104672612 B CN104672612 B CN 104672612B
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temperature
area
polypropylene material
screw extruder
double screw
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CN104672612A (en
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葛卫平
陈宗美
王维根
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Nanjing Valley Intellectual Property Service Co., Ltd.
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Nanjing Valley Intellectual Property Service Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a flame retardant polypropylene material and a preparation method thereof. The polypropylene material is prepared from the following components in parts by weight: 85-93 parts of polypropylene resin, 12-15 parts of glass fiber, 5-8 parts of kieselguhr, 2-3 parts of azodiisobutyronitrile, 0.8-2 parts of a fire retardant, 0.5-1.4 parts of polyepoxysuccinic acid and 0.05-1 part of antioxygen. The invention also provides the preparation method of the flame retardant polypropylene material. The method comprises the following steps: placing the materials in a high speed mixer to uniformly mix, mixing the uniformly mixed materials for 5-10 minutes in a double-roller open mill at the mixing temperature of 170-190 DEG C, adding the mixed materials to a charging port of a double-screw extruder for melt extrusion by the double-screw extruder, and pelleting to prepare the flame retardant polypropylene material.

Description

A kind of anti-flaming polypropylene material and preparation method thereof
Technical field
The invention belongs to polymeric material field, particularly to a kind of anti-flaming polypropylene material and preparation method thereof.
Background technology
Polypropylene is polymer nontoxic, that odorless, tasteless milky are highly crystalline.It is particularly stable to water, good moldability, Easy processing and cheap, is widely used in the industries such as chemical industry, chemical fibre, packaging, household electrical appliances.But, polypropylene exists high temperature resistant strong Degree is not enough and inflammable the shortcomings of be easily fuming, and which greatly limits the range of application of polypropylene material.
Polypropylene modified material can discharge some irritative gass, to varying degrees with people's ring during using Protect the enhancing of health perception, polypropylene material is faced with huge challenge.In order to expand polypropylene material further in related neck The application in domain, prepared polypropylene material does not need only have good performance, is also required to possess environmental protection characteristic simultaneously.
Flame-retardant system has reached its maturity, and modal fire retardant systems have halogen system compound, halogen system compound and auxiliary Fire retardant to improve flame retardant effect jointly.Due to there being halogen fire retardant all can produce large effect to environment and personal safety, because And limit its application in each field
Patent CN103965636A discloses a kind of automotive plastic parts polypropylene flame redardant modified polyphenyl thioether material, passes through Glass fibre, polypropylene, kieselguhr, magnesium oxide, accelerant B PP, flyash, aminopropyl-triethoxy is added in polyphenylene sulfide The components such as silane, beryllium oxide, prepared polypropylene material combines the advantage of the raw materials such as polyphenylene sulfide, polypropylene, glass fibre, There is good processing characteristics and mechanical performance, but its fire resistance not good it is impossible to meet electronic equipment casing for fire-retardant Require.
Content of the invention
For above-mentioned demand, invention especially provides a kind of anti-flaming polypropylene material and preparation method thereof.The present invention Anti-flaming polypropylene material there is good high temperature resistant and weather resistance, can and high temperature this moist in cleaning shop environment In, the good mechanical property of long-term holding.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of anti-flaming polypropylene material, is made up of the component comprising following weight portion：
Acrylic resin 85-93 part,
Glass fibre 12-15 part,
Kieselguhr 5-8 part,
Azodiisobutyronitrile 2-3 part,
Fire retardant 0.8-2 part,
Poly-epoxy succinic acid 0.5-1.4 part,
Antioxidant 0.05-1 part.
Described fire retardant is the mixed of one or more of sodium tripolyphosphate, aluminium oxide and isocyanuric acid three-glycidyl ester Close.
Described fire retardant is sodium tripolyphosphate, aluminium oxide, the mixture of isocyanuric acid three-glycidyl ester, described trimerization phosphorus Sour sodium, aluminium oxide, the mass ratio of isocyanuric acid three-glycidyl ester are 1:1:2.
Described antioxidant be selected from four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propanoic acid] pentaerythritol ester or three ［ 2.4- Di-tert-butyl-phenyl ］ one of phosphite ester or two kinds mixing.
A kind of preparation method of anti-flaming polypropylene material, the method comprises the following steps：
（1）Weigh acrylic resin 85-93 part, glass fibre 12-15 part, kieselguhr 5-8 part, azodiisobutyronitrile 2-3 Part, fire retardant 0.8-2 part, poly-epoxy succinic acid 0.5-1.4 part and antioxidant 0.05-1 part；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 5-10 minute, melting temperature is 170-190 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material.
One area's temperature of described double screw extruder is 160-180 DEG C, and two area's temperature are 190-230 DEG C, and three area's temperature are 230-240 DEG C, four area's temperature are 210-220 DEG C, and five area's temperature are 180-200 DEG C, and head temperature is 220-230 DEG C, and main frame turns Speed is 15-35HZ.
Compared with prior art, its advantage is the present invention：
（1）The anti-flaming polypropylene material of the present invention passes through to add kieselguhr and compounding fire retardant, prepared polypropylene material Material has good mechanical property and fire resistance, and resistance to elevated temperatures is good, is not added with aldehydes and ketone in preparation process , thus there is not corresponding potential safety hazard in material.
（2）The anti-flaming polypropylene material that the present invention is obtained passes through to add poly-epoxy succinic acid so as in different use rings Remain to keep good stability and weatherability in border.
（3）The anti-flaming polypropylene material of the present invention, its preparation method simple it is easy to industrialized production.
Specific embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1
（1）Weigh acrylic resin 85kg, glass fibre 15kg, kieselguhr 5kg, azodiisobutyronitrile 2kg, tripolyphosphate Sodium 0.8kg, poly-epoxy succinic acid 0.5kg and four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propanoic acid] pentaerythritol ester 0.05kg；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 5 minutes, melting temperature is 170 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material,
Wherein, area's temperature of described double screw extruder is 160 DEG C, and two area's temperature are 190 DEG C, and three area's temperature are 230 DEG C, four area's temperature are 210 DEG C, and five area's temperature are 180 DEG C, and head temperature is 220 DEG C, and engine speed is 15HZ.
The performance test results of prepared anti-flaming polypropylene material are as shown in table 1.
Embodiment 2
（1）Weigh acrylic resin 85kg, glass fibre 12kg, kieselguhr 5kg, azodiisobutyronitrile 2kg, isocyanuric acid Three-glycidyl ester 0.8kg, poly-epoxy succinic acid 0.5kg and four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propanoic acid] season penta Four alcohol ester 0.05kg；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 5 minutes, melting temperature is 170 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material,
Wherein, area's temperature of described double screw extruder is 160 DEG C, and two area's temperature are 190 DEG C, and three area's temperature are 230 DEG C, four area's temperature are 210 DEG C, and five area's temperature are 180 DEG C, and head temperature is 220 DEG C, and engine speed is 15HZ.
The performance test results of prepared anti-flaming polypropylene material are as shown in table 1.
Embodiment 3
（1）Weigh acrylic resin 93kg, glass fibre 15kg, kieselguhr 5kg, azodiisobutyronitrile 3kg, tripolyphosphate Sodium 0.5kg, aluminium oxide 0.5kg, isocyanuric acid three-glycidyl ester 1kg, poly-epoxy succinic acid 1.4kg and three ［ the tertiary fourth of 2.4- bis- Base phenyl ］ phosphite ester 1kg；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 10 minutes, melting temperature is 190 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material,
Wherein, area's temperature of described double screw extruder is 180 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, four area's temperature are 220 DEG C, and five area's temperature are 200 DEG C, and head temperature is 230 DEG C, and engine speed is 35HZ.
The performance test results of prepared anti-flaming polypropylene material are as shown in table 1.
Embodiment 4
（1）Weigh acrylic resin 93kg, glass fibre 15kg, kieselguhr 8kg, azodiisobutyronitrile 3kg, tripolyphosphate Sodium 0.5kg, aluminium oxide 0.5kg, isocyanuric acid three-glycidyl ester 1kg, poly-epoxy succinic acid 1.4kg and three ［ the tertiary fourth of 2.4- bis- Base phenyl ］ phosphite ester 0.5kg；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 10 minutes, melting temperature is 190 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material,
Wherein, area's temperature of described double screw extruder is 180 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, four area's temperature are 220 DEG C, and five area's temperature are 200 DEG C, and head temperature is 230 DEG C, and engine speed is 35HZ.
The performance test results of prepared anti-flaming polypropylene material are as shown in table 1.
Embodiment 5
（1）Weigh acrylic resin 90kg, glass fibre 14kg, kieselguhr 6kg, azodiisobutyronitrile 2kg, tripolyphosphate Sodium 0.25kg, aluminium oxide 0.25kg, isocyanuric acid three-glycidyl ester 0.5kg, poly-epoxy succinic acid 1kg, four [β-（3,5- bis- Tert-butyl-hydroxy phenyl）Propanoic acid] pentaerythritol ester 0.25kg and three ［ 2.4- di-tert-butyl-phenyl ］ phosphite ester 0.25kg；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, by the material of mix homogeneously in two-roll mill Carry out kneading 7 minutes, melting temperature is 180 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, make Grain, prepares anti-flaming polypropylene material,
Wherein, area's temperature of described double screw extruder is 170 DEG C, and two area's temperature are 215 DEG C, and three area's temperature are 235 DEG C, four area's temperature are 215 DEG C, and five area's temperature are 190 DEG C, and head temperature is 225 DEG C, and engine speed is 20HZ.
The performance test results of prepared anti-flaming polypropylene material are as shown in table 1.
Comparative example
Weigh acrylic resin 90kg, glass fibre 14kg, kieselguhr 6kg, azodiisobutyronitrile 2kg, sodium tripolyphosphate 0.25kg, aluminium oxide 0.25kg, decabromodiphenyl oxide 0.5kg and three ［ 2.4- di-tert-butyl-phenyl ］ phosphite ester 0.25kg, mixing Uniformly, the material of mix homogeneously is carried out in two-roll mill knead 10 minutes, melting temperature is 180 DEG C, after mixing Material adds the charge door of double screw extruder, melt extrudes through double screw extruder, pelletize, prepares polypropylene material, Wherein, area's temperature of described double screw extruder is 180 DEG C, and two area's temperature are 200 DEG C, and three area's temperature are 215 DEG C, four area's temperature Spend for 210 DEG C.
Table 1

Claims (2)

1. a kind of anti-flaming polypropylene material is it is characterised in that be made up of the component comprising following weight portion：
Acrylic resin 85-93 part,
Glass fibre 12-15 part,
Kieselguhr 5-8 part,
Azodiisobutyronitrile 2-3 part,
Fire retardant 0.8-2 part,
Poly-epoxy succinic acid 0.5-1.4 part,
Antioxidant 0.05-1 part；
Described fire retardant is sodium tripolyphosphate, aluminium oxide, the mixture of isocyanuric acid three-glycidyl ester, described tripolyphosphate Sodium, aluminium oxide, the mass ratio of isocyanuric acid three-glycidyl ester are 1:1:2；
Described antioxidant be selected from four [β-（3,5- di-t-butyl -4- hydroxy phenyls）Propanoic acid] pentaerythritol ester or three ［ 2,4- Di-tert-butyl-phenyl ］ one of phosphite ester or two kinds mixing；
A kind of described anti-flaming polypropylene material is prepared by following preparation methoies：
（1）Weigh acrylic resin 85-93 part, glass fibre 12-15 part, kieselguhr 5-8 part, azodiisobutyronitrile 2-3 Part, fire retardant 0.8-2 part, poly-epoxy succinic acid 0.5-1.4 part and antioxidant 0.05-1 part；
（2）Above-mentioned material is put into mix homogeneously in high-speed mixer, the material of mix homogeneously is carried out in two-roll mill Mixing 5-10 minute, melting temperature is 170-190 DEG C；
（3）Material after mixing is added the charge door of double screw extruder, melt extrude through double screw extruder, pelletize, system Standby obtain anti-flaming polypropylene material.
2. a kind of anti-flaming polypropylene material according to claim 1 is it is characterised in that an area of described double screw extruder Temperature is 160-180 DEG C, and two area's temperature are 190-230 DEG C, and three area's temperature are 230-240 DEG C, and four area's temperature are 210-220 DEG C, Five area's temperature are 180-200 DEG C, and head temperature is 220-230 DEG C, and engine speed is 15-35Hz.
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CN108997649A (en) * 2018-06-22 2018-12-14 宁波蒙曼生物科技有限公司 A kind of anti-flaming polypropylene material and its preparation and application
CN109942846B (en) * 2019-03-27 2022-02-01 山东润科化工股份有限公司 Tetrabromobisphenol A bis (2, 3-dibromo-2-methylpropyl) ether flame-retardant master batch and preparation method thereof
CN112759835B (en) * 2020-12-30 2022-06-28 宁波市北仑区德恒模塑有限公司 High polymer material for toy and preparation equipment thereof

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CN101412830A (en) * 2008-12-02 2009-04-22 上海金发科技发展有限公司 Non-halogen flame-retardant polypropylene composite material and preparation thereof
CN102040775A (en) * 2010-12-24 2011-05-04 洛阳市河之阳高分子材料有限公司 Flame retardant polypropylene material
CN102492218B (en) * 2011-11-29 2013-10-23 深圳市科聚新材料有限公司 Halogen-free expansion type flame-retardant glass fiber reinforced polypropylene material and preparation method thereof
CN102516667A (en) * 2011-12-19 2012-06-27 江苏金发科技新材料有限公司 Halogen-free flame-retardant long glass fiber reinforced polypropylene material and preparation method thereof
CN103849068A (en) * 2012-12-04 2014-06-11 青岛三利中德美水设备有限公司 Glass fiber-reinforced halogen-free flame retardant PP(Polypropylene)/PE(Polyethylene) alloy material and preparation method thereof
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CN104098836A (en) * 2014-06-27 2014-10-15 广东威林工程塑料有限公司 Halogen-free flame-retardant reinforced polypropylene material containing polyamide charring agent and preparation method thereof
CN104212061B (en) * 2014-09-12 2016-05-04 河南科技大学 A kind of high-strength abrasion-proof polypropylene flame redardant and preparation method thereof

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