CN110734608A - flame-retardant master batch and application thereof in flame-retardant polypropylene material - Google Patents

flame-retardant master batch and application thereof in flame-retardant polypropylene material Download PDF

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Publication number
CN110734608A
CN110734608A CN201911034423.4A CN201911034423A CN110734608A CN 110734608 A CN110734608 A CN 110734608A CN 201911034423 A CN201911034423 A CN 201911034423A CN 110734608 A CN110734608 A CN 110734608A
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flame
retardant
polypropylene
master batch
base material
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刘春晓
张雪
刘平平
车雪梅
从文韬
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Yantai Geruien Polymer Materials Co Ltd
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Yantai Geruien Polymer Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10Homopolymers or copolymers of propene
    • C08J2323/12Polypropene
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04Homopolymers or copolymers of ethene
    • C08J2423/06Polyethene
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04Homopolymers or copolymers of ethene
    • C08J2423/08Copolymers of ethene
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10Homopolymers or copolymers of propene
    • C08J2423/12Polypropene
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10Homopolymers or copolymers of propene
    • C08J2423/14Copolymers of propene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/02Halogenated hydrocarbons
    • C08K5/03Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses flame-retardant master batches, which comprise, by weight, 8-10 parts of a polypropylene base material, 4-5 parts of a low-density polyethylene base material, 70-85 parts of a flame retardant, 2-5 parts of a toughening agent, 0.5-0.8 part of an antioxidant, 0.5-0.7 part of a lubricant and 0.8-1 part of a light stabilizer.

Description

flame-retardant master batch and application thereof in flame-retardant polypropylene material
Technical Field
The invention relates to a flame-retardant material, in particular to flame-retardant master batches and application thereof in a flame-retardant polypropylene material.
Background
With the increasing updating speed of electronic and electric products, people have an increasing interest in the safety performance of the electronic and electric products while the functional requirements of the products are improved. Recently, accidents such as mobile phone explosion, television explosion, spontaneous combustion of electric vehicles and spontaneous combustion of new energy vehicles frequently occur, and the accidents not only cause property loss, but also cause casualties. Therefore, flame retardant treatment of electronic and electric products is imperative.
The polypropylene material is common plastic used in electronic and electric appliance shells and interior decorations, the oxygen index is about 17 percent, the polypropylene material belongs to flammable materials, the high crystallinity and the inflammability of the polypropylene limit the safe application of the polypropylene material in the electronic and electric appliance industry, the addition of the flame retardant can solve the safe limitation of the application of the polypropylene material in the electronic and electric appliance industry, but most of the flame retardants are powder with the particle size of over 800 meshes, the dispersibility in the polypropylene material is poor, the phenomena of screw slipping, dust raising, unsmooth extruded material surface, white spots and the like are easy to occur in the processing process, the flame retardant efficiency is low, the addition amount of the traditional bromine antimony flame retardant is which is over 5 percent, and the smoke generation amount of flame retardant high molecular products is large when the flame retardant is burnt.
Disclosure of Invention
Aiming at the problem of poor flame retardant effect of the conventional flame retardant for polypropylene, the invention provides flame-retardant master batches and application thereof in flame-retardant polypropylene materials.
The technical scheme for solving the technical problems is that flame-retardant master batches are characterized by comprising, by weight, 8-10 parts of polypropylene base material, 4-5 parts of low-density polyethylene base material, 70-85 parts of flame retardant, 2-5 parts of flexibilizer, 0.5-0.8 part of antioxidant, 0.5-0.7 part of lubricant and 0.8-1 part of light stabilizer.
The polypropylene base material is or two of homo-polypropylene or co-polypropylene, the melt index of the polypropylene base material is 20-30g/10min, the melt index of the polypropylene base material is 230 ℃ and 2.16 kg., and the melt index of the low-density polyethylene base material is 2-3g/10min, the melt index of the low-density polyethylene base material is 190 ℃ and 2.16 kg.
The flame retardant comprises, by weight, 35-40% of decabromodiphenylethane, 10-20% of silicate compounds and 40-55% of phosphorus-nitrogen flame retardants, wherein the whiteness of the decabromodiphenylethane is 92-93, the particle size of the silicate compounds is less than 5 mu m, and the phosphorus-nitrogen flame retardants are or more of ammonium polyphosphate, aluminum diethylphosphinate, aluminum hypophosphite or melamine polyphosphate.
The toughening agent is a mixture of 1:1 of an ethylene-octene copolymer and an ethylene-butene copolymer; the antioxidant is Basff 1010; the lubricant is N, N' -ethylene bis stearamide; the light stabilizer is basf Tinuvin770 DF.
The flame-retardant master batch can be used for preparing flame-retardant polypropylene materials, and the preparation method comprises the following steps:
1) preparing master batch: weighing the components of the flame-retardant master batch according to the weight parts, adding the polypropylene base material, the low-density polyethylene base material, the flame retardant, the toughening agent, the antioxidant, the lubricant and the light stabilizer into a high-speed mixing machine for mixing for 10min, uniformly mixing, melting, mixing and extruding by a double-screw extruder, cooling by water, drying, and then granulating in a granulator to obtain the flame-retardant master batch;
2) preparing a flame-retardant polypropylene material: and (2) uniformly mixing the flame-retardant master batch obtained in the step 1) with the polypropylene body, performing melt mixing extrusion by using a double-screw extruder, performing water cooling and drying, and then performing granulation in a granulator to obtain the flame-retardant polypropylene composite material.
In the step 1), the temperature of the high-speed mixing machine is 110-.
The invention has the beneficial effects that: the flame-retardant master batch has the advantages of less consumption in the body, about 1-3%, less influence on the mechanical property of the body, good compatibility with polypropylene materials, and avoidance of adverse phenomena of screw slipping, unsmooth material surface and the like caused by uneven grain powder in the extrusion process of flame-retardant polypropylene products, the polypropylene materials for electronic and electric appliances subjected to flame-retardant treatment by the flame-retardant master batch of the invention conform to UL94V-2(1.5mm), pass glow wire tests of GWIT750 ℃ (0.75mm) and GWIT 850 ℃ (0.75mm), and avoid the problem of dust pollution easily caused by flame retardants.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
flame-retardant master batches, which are composed of the components shown in Table 1:
TABLE 1 flame retardant masterbatch proportioning (kg) of example 1
Homo-polypropylene 10
Low density polyethylene 4
Decabromodiphenylethane 32
Potassium silicate 8
Ammonium polyphosphate 40
Toughening agent 4
Pasteur antioxidant 1010 0.5
N, N' -ethylene bis stearamide 0.5
Tenf Tinuvin770DF 1
In Table 1, the melt index of the homo-polypropylene is 20g/10min, 230 ℃ and 2.16kg, and the melt index of the low-density polyethylene base material is 3g/10min, 190 ℃ and 2.16 kg; the toughening agent is a 1:1 mixture of ethylene-octene copolymer and ethylene-butene copolymer.
The method for preparing the flame-retardant polypropylene material by adopting the flame-retardant master batch comprises the steps of 1) accurately weighing raw materials according to the ratio, adding all times into a high-speed mixing machine for mixing for 10min, transferring the uniformly mixed materials into a feed hopper of a double-screw extruder, controlling the temperature of a region of the double-screw extruder to be 185 ℃, the temperature of a second region to be 200 ℃, the temperature of a third region to be 205 ℃, the temperature of a fourth region to be 210 ℃, the temperature of a machine head to be 220 ℃, carrying out melt mixing extrusion by the double-screw extruder, controlling the residence time before extrusion to be 3min, drawing by a tractor to enter a water cooling tank and a dryer, controlling the drawing speed to be 5m/min, drying, and then entering a granulator for granulation to obtain the flame-retardant master batch, and 2) uniformly mixing the polypropylene base material for the electronic appliance and the flame-retardant master batch according to the ratio of 98:2, then sending the.
Example 2
flame-retardant master batches, which are composed of the components shown in Table 2:
TABLE 2 EXAMPLE 2 flame retardant masterbatch proportioning (kg)
Polypropylene copolymer 8
Low density polyethylene 5
Decabromodiphenylethane 33.12
Manganese silicate 8.28
Ammonium polyphosphate 41.4
Toughening agent 2
Pasteur antioxidant 1010 0.8
N, N' -ethylene bis stearamide 0.6
Tenf Tinuvin770DF 0.8
In Table 2, the melt index of the homo-polypropylene is 25g/10min, 230 ℃ and 2.16kg, and the melt index of the low-density polyethylene base material is 2.5g/10min, 190 ℃ and 2.16 kg; the toughening agent is a 1:1 mixture of ethylene-octene copolymer and ethylene-butene copolymer.
The method for preparing the flame-retardant polypropylene material by adopting the flame-retardant master batch comprises the steps of 1) accurately weighing raw materials according to the ratio, adding all times into a high-speed mixing machine for mixing for 10min, transferring the uniformly mixed materials into a feed hopper of a double-screw extruder, controlling the temperature of a region of the double-screw extruder to be 170 ℃, the temperature of a second region to be 190 ℃, the temperature of a third region to be 200 ℃, the temperature of a fourth region to be 200 ℃, the temperature of a machine head to be 210 ℃, carrying out melt mixing extrusion by the double-screw extruder, controlling the residence time before extrusion to be 5min, drawing by a tractor to enter a water cooling tank and a dryer, controlling the drawing speed to be 5m/min, drying, and then entering a granulator for granulation to obtain the flame-retardant master batch, and 2) uniformly mixing the polypropylene base material for the electronic appliance and the flame-retardant master batch according to the ratio of 99:1, then feeding.
Example 3
flame-retardant master batches, which are composed of the components shown in Table 3:
TABLE 3 EXAMPLE 3 flame retardant masterbatch proportioning (kg)
Homo-polypropylene 5
Polypropylene copolymer 5
Low densityPolyethylene of high degree 5
Decabromodiphenylethane 31.2
Sodium silicate 7.8
Ammonium polyphosphate 39
Toughening agent 4.6
Pasteur antioxidant 1010 0.7
N, N' -ethylene bis stearamide 0.7
Tenf Tinuvin770DF 1
In Table 3, the melt index of the homo-polypropylene is 30g/10min, 230 ℃ and 2.16kg, the melt index of the co-polypropylene is 20g/10min, 230 ℃ and 2.16kg, and the melt index of the low-density polyethylene substrate is 2g/10min, 190 ℃ and 2.16 kg; the toughening agent is a 1:1 mixture of ethylene-octene copolymer and ethylene-butene copolymer.
The method for preparing the flame-retardant polypropylene material by adopting the flame-retardant master batch comprises the steps of 1) accurately weighing the raw materials according to the ratio, adding all times into a high-speed mixing machine for mixing for 10min, transferring the uniformly mixed materials into a feed hopper of a double-screw extruder, wherein the temperature of a region of the double-screw extruder is 175 ℃, the temperature of a two region is 210 ℃, the temperature of a three region is 204 ℃, the temperature of a four region is 205 ℃, the temperature of a machine head is 215 ℃, carrying out melt mixing extrusion by the double-screw extruder, keeping the residence time before extrusion for 4min, drawing by a tractor into a water cooling tank and a dryer at the drawing speed of 5m/min, drying, and then feeding into a granulator for granulation to obtain the flame-retardant master batch, and 2) uniformly mixing the polypropylene base material for the electronic appliance and the flame-retardant master batch according to the ratio of 97:3, feeding into the feed hopper of the double-.
The flame-retardant polypropylene materials obtained in examples 1 to 3 and the conventional non-flame-retardant polypropylene materials were prepared into standard sample strips, and the results thereof are shown in Table 4.
TABLE 4 test results of the flame retardant polypropylene materials obtained in examples 1 to 3 and the conventional polypropylene materials
Figure BDA0002251058920000061
Remarking:
1. test standard
Vertical burning test: ANSI/UL-94-1985;
glow wire flammability test of materials: GB/T5169.12-2013;
glow wire ignition test of the materials: GB/T5169.13-2013;
the smoke density test method comprises the following steps: GB/T20284-2006.
2. "√" indicates a pass test; "X" indicates failure of the test.
As shown by comparative analysis of test data in Table 4, after the flame-retardant master batch is used in the polypropylene material for electronic and electric appliances, the material can reach UL94V-2(1.5mm), and the smoke generation rate index does not exceed 30m2/s2While passing the GWIT750 ℃ (0.75mm) GWFI 850 ℃ (0.75mm) glow wire test.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1, flame-retardant master batches, which are characterized by comprising the following components in parts by weight:
8-10 parts of polypropylene base material, 4-5 parts of low-density polyethylene base material, 70-85 parts of flame retardant, 2-5 parts of toughening agent, 0.5-0.8 part of antioxidant, 0.5-0.7 part of lubricant and 0.8-1 part of light stabilizer.
2. The flame-retardant masterbatch according to claim 1, wherein the polypropylene base material is kinds or two kinds of homo-polypropylene or co-polypropylene, and its melt index is 20-30g/10min, 230 ℃, 2.16 kg.
3. The flame retardant masterbatch according to claim 1, wherein the low density polyethylene base material has a melt index of 2-3g/10min, 190 ℃, 2.16 kg.
4. The flame retardant masterbatch according to claim 1, wherein the flame retardant comprises the following components by weight: 35-40% of decabromodiphenylethane, 10-20% of silicate compound and 40-55% of phosphorus-nitrogen flame retardant;
the whiteness of the decabromodiphenylethane is 92-93;
the particle size of the silicate compound is less than 5 mu m;
the phosphorus-nitrogen flame retardant is or more of ammonium polyphosphate, aluminum diethylphosphinate, aluminum hypophosphite or melamine polyphosphate.
5, flame-retardant polypropylene material, which is characterized in that the flame-retardant polypropylene material is composed of the flame-retardant master batch of any of claims 1-4 and a polypropylene body, and the preparation method comprises the following steps:
1) preparing master batch: weighing the components of the flame-retardant master batch according to the weight parts, adding the polypropylene base material, the low-density polyethylene base material, the flame retardant, the toughening agent, the antioxidant, the lubricant and the light stabilizer into a high-speed mixing machine for mixing for 10min, uniformly mixing, melting, mixing and extruding by a double-screw extruder, cooling by water, drying, and then granulating in a granulator to obtain the flame-retardant master batch;
2) preparing a flame-retardant polypropylene material: uniformly mixing the flame-retardant master batch obtained in the step 1) with the polypropylene body, performing melt mixing extrusion by a double-screw extruder, performing water cooling and drying, and then performing granulation in a granulator to obtain the flame-retardant polypropylene composite material.
6. The flame retardant polypropylene material according to claim 5, wherein in the step 1), the temperature of the high speed mixer is 100-.
7. The flame-retardant polypropylene material according to claim 5, wherein in the step 1), the temperature of the zone of the twin-screw extruder is 160-.
8. The flame retardant polypropylene material according to claim 5, wherein in the step 2), the proportion of the flame retardant master batch in the flame retardant polypropylene material is 1-3 wt%.
9. The flame-retardant polypropylene material according to claim 5, wherein in the step 2), the temperature of the zone of the twin-screw extruder is 160-.
CN201911034423.4A 2019-10-29 2019-10-29 flame-retardant master batch and application thereof in flame-retardant polypropylene material Pending CN110734608A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111499962A (en) * 2020-05-27 2020-08-07 广东聚石化学股份有限公司 anti-UV halogen-free flame-retardant master batch and preparation method and application thereof
CN112063044A (en) * 2020-08-19 2020-12-11 上海金发科技发展有限公司 Flame-retardant polypropylene composition capable of preventing pet from biting and preparation method thereof
CN115058079A (en) * 2022-05-05 2022-09-16 清远市一丞阻燃材料有限公司 Preparation method of flame-retardant polypropylene

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CN102241857A (en) * 2010-09-25 2011-11-16 深圳市科聚新材料有限公司 Polypropylene flame-retardant masterbatch material and preparation method thereof

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CN102241857A (en) * 2010-09-25 2011-11-16 深圳市科聚新材料有限公司 Polypropylene flame-retardant masterbatch material and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111499962A (en) * 2020-05-27 2020-08-07 广东聚石化学股份有限公司 anti-UV halogen-free flame-retardant master batch and preparation method and application thereof
CN112063044A (en) * 2020-08-19 2020-12-11 上海金发科技发展有限公司 Flame-retardant polypropylene composition capable of preventing pet from biting and preparation method thereof
CN115058079A (en) * 2022-05-05 2022-09-16 清远市一丞阻燃材料有限公司 Preparation method of flame-retardant polypropylene

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Application publication date: 20200131