CN107857938A - A kind of halogen-free anti-flaming polypropylene material and its preparation method and application - Google Patents
A kind of halogen-free anti-flaming polypropylene material and its preparation method and application Download PDFInfo
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- CN107857938A CN107857938A CN201711231372.5A CN201711231372A CN107857938A CN 107857938 A CN107857938 A CN 107857938A CN 201711231372 A CN201711231372 A CN 201711231372A CN 107857938 A CN107857938 A CN 107857938A
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- halogen
- polypropylene material
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- flaming polypropylene
- antimony oxide
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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
- 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
- C08L23/14—Copolymers of propene
-
- 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
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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
Abstract
The invention belongs to technical field of polymer materials, is related to a kind of halogen-free anti-flaming polypropylene material and its preparation method and application.The halogen-free anti-flaming polypropylene material includes following components in percentage by weight:HOPP:32.4~45.4%, COPP:30~35%, antimony oxide:7~8%, nitrogen phosphorus fire retardant:16~22%, antioxidant:0.8~1.6%, processing aid:0.8~1.0%.Each component is weighed according to above-mentioned percentage by weight, after being well mixed, is added in double screw extruder, extruding pelletization obtains halogen-free anti-flaming polypropylene material, can be used for preparing the Plastic Drum for accommodating inflammability solid, liquid or gas.
Description
Technical field
The invention belongs to technical field of polymer materials, be related to a kind of halogen-free anti-flaming polypropylene material and preparation method thereof and
Using.
Background technology
Polypropylene (PP) is a kind of thermoplastic, and its light specific gravity, finished surface hardness is big, and elasticity is high, heat resistance, chemistry
Stability, insulating properties are good, are widely used in numerous areas, are the plastics varieties for being most hopeful to realize general-purpose plastics engineering
One of.Because the propylene monomer that polypropylene is made up of carbon hydrogen element is polymerized, its molecular structure determines common gather
Propylene material does not have anti-flammability, meets fire and fires, and limited oxygen index (LOI) is only 17.4-18.5, and molten drop is serious during burning,
Easy propagating flame causes fire, and these defects make it unsafe factor in application process be present.Require high in fire-retardant condition
Environment in, as being used for of preparing of PP materials accommodates the Plastic Drum of inflammability solid, liquid or gas, PP must just be changed
Property, it is allowed to meet flame-retarding characteristic requirement.Presently mainly PP fire resistance is improved by adding fire retardant.
With the continuous reinforcement of people's environmental consciousness, the environmental requirement for flame retardant products is also more and more stricter.It is halogen
Though fire retardant and material compatibility be good, small to the performance impact of material, due to it, in burning, smoke amount is big, produces halogenation
The substantial amounts of toxic gas such as hydrogen, and be possible to produce carcinogenic bioxin, to mankind itself and its environmental danger, thus
Increasing people transfers to select halogen-free flame retardants.
Nitrogen phosphorus fire retardant has higher flame retardant effect, excellent heat endurance because of the cooperative effect of nitrogen phosphorus, extensive
Applied to the flame retardant treatment of the engineering plastics such as PBT, PA66, ABS, antimony oxide (Sb is added in nitrogen phosphorus fire retardant2O3),
Sb2O3As flame retardant, the fire resistance of nitrogen phosphorus fire retardant can further improve.But antimony oxide and nitrogen phosphorus fire retardant
Optimal collaboration proportioning is in response to different and different with matrix, and the proportioning of the two compares and significantly affected between fire retardant and matrix
Compatibility, so as to influence the mechanical property of the performance of fire retardant effect and material.
The content of the invention
It is an object of the invention to provide a kind of halogen-free anti-flaming polypropylene material, the PP materials have excellent flame retardant effect, resisted
Oxidisability and mechanical property, and the method for preparing the PP materials is simple, practicality is extremely strong, and is easily achieved industrialized production.
In order to reach foregoing invention purpose, the present invention uses following technical scheme:A kind of halogen-free anti-flaming polypropylene material, institute
Stating halogen-free anti-flaming polypropylene material includes following components in percentage by weight:
HOPP:32.4~45.4%,
COPP:30~35%,
Antimony oxide:7~8%,
Nitrogen phosphorus fire retardant:16~22%,
Antioxidant:0.8~1.6%,
Processing aid:0.8~1.0%.
The present invention uses the matrix of HOPP and COPP as halogen-free anti-flaming polypropylene material so that matrix
With good mechanical property, using antimony oxide and nitrogen phosphorus fire retardant as fire retardant, the two cooperative flame retardant effect is played.
By constantly research and development, each component optimization formula ratio is obtained, each component is under above-mentioned optimization formula ratio, fire retardant and polypropylene compatible
Property is preferable, and the synergy compounded between fire retardant is preferable.
The nitrogen phosphorus fire retardant is fire-retardant from the model QB-B01 of Shijiazhuang Qi Bo Chemical Co., Ltd.s production nitrogen phosphorus
Agent.
Preferably, the weight of the HOPP and COPP ratio is (1.1-1.5):1.HOPP and
COPP is used in combination according to the proportioning of the present invention, the two complex network structures formed, improves the mechanical property of material,
And make it that nitrogen phosphorus fire retardant and antimony oxide are dispersed in this complex network structures, improve mutual compatible
Property.
Preferably, the weight ratio of the nitrogen phosphorus fire retardant and antimony oxide is (2.2-2.8):1.Sb2O3In burning just
Phase, it is melting first, forms diaphragm isolation air in material surface, by the internal endothermic reaction, reduce ignition temperature, simultaneously
Antimony oxide is gasified at high operating temperatures, dilutes oxygen concentration in air, so as to play fire retardation.Nitrogen phosphorus fire retardant because
Synergy between element has good fire retardation with acting synergistically.For theory, antimony oxide and nitrogen phosphorus fire retardant are simultaneously
With, easily produce N-P-Sb cooperative effects, improve the flame retardant effect and mechanical property of material, but in practical operation, it is necessary to
Consider Sb2O3With the compatibility of nitrogen phosphorus fire retardant and matrix material.The two makes the two and poly- third using the weight ratio in the present invention
The compatibility of alkenyl body improves, and at utmost plays flame retardant synergistic effect.
Preferably, the antimony oxide, which is cyclodextrin, wraps up antimony oxide.Cyclodextrin is particularly ring-shaped structure,
It has hydrophobic cavity, and antimony oxide is easily accessible cyclodextrin hydrophobic cavity, the ring of formation by special preparation method
Dextrin coats antimony oxide because the hydrophilic bond of particle surface cyclodextrin is present, so as to substantially increase its phase with material matrix
Capacitive, strengthen the cooperative effect of antimony oxide and nitrogen phosphorus fire retardant.In addition, cyclodextrin is because of its particularly ring-shaped structure, from
Body just has good carbon-forming performance and thermal stability, so as to further increase the flame retardant effect of fire retardant.
Preferably, the preparation method of the cyclodextrin parcel antimony oxide is:Cyclodextrin is scattered in ethanol,
3000~5000r/min stirs 20~40min, then heats to 80~100 DEG C, adds antimony oxide, 300~500r/min
Lasting stirring, 3~5h of insulation reaction, filtering, washing, dry.The cyclodextrin is beta-schardinger dextrin, contains 6-12 glucose list
Member.By the preparation method antimony oxide of the present invention in cyclodextrin ethanol suspension, easily into the thin of cyclodextrin
Water cavity, so as to form cyclodextrin parcel antimony oxide.
Preferably, the mol ratio of the cyclodextrin and antimony oxide is (1.2-1.5):1.The amount of cyclodextrin very little,
Can not fully wrapped around antimony oxide, free antimony oxide, which remains unchanged, can influence the compatibility of fire retardant and matrix;Cyclodextrin
Amount is too many, and after fully wrapped around antimony oxide, unnecessary cyclodextrin continues to deposit onto antimony oxide surface, forms thick one
Cyclodextrin layer, influences flame retardant effect.
Preferably, the antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 1135, antioxidant 1098, antioxygen
One or more in agent 168, anti-oxidant DLTP.Further preferably, described antioxidant is irgasfos 168 and anti-oxidant DLTP
Compounding, the mass ratio (1~2) of irgasfos 168 and anti-oxidant DLTP:1.
Preferably, the processing aid is one kind in PE waxes, ethylene bis stearamide (EBS), calcium stearate, silicone
It is or a variety of.
In order to reach another object of the present invention, adopt the following technical scheme that:A kind of halogen-free anti-flaming polypropylene material
Preparation method, the preparation method include:Each component is weighed according to percentage by weight, after being well mixed, adds double screw extruder
In, extruding pelletization;Wherein, double screw extruder engine speed 25-31HZ, temperature are 210-230 DEG C.
4-6min is mixed in the high speed mixer that rotating speed is 400-600rmp/min after each component is weighed, makes each component
It is well mixed.
A kind of application of halogen-free anti-flaming polypropylene material in the Plastic Drum for accommodating combustible material.Especially, the Halogen hinders
Polypropylene material is fired to be applied in the Plastic Drum of receiving sodium hydrosulfite (sodium dithionite).
The present invention uses HOPP and COPP as matrix, antimony oxide and nitrogen phosphorus fire retardant as resistance
Agent is fired, under optimal proportion of the present invention, compatibility is good between each composition, and material mechanical performance is good, flame retardant effect is good, can be well
Applied in the Plastic Drum for accommodating combustible material.
Embodiment
Explanation is further described to technical scheme below by specific embodiment.If without specified otherwise,
Raw material employed in embodiments of the invention is raw material commonly used in the art, the method employed in embodiment, is this
The conventional method in field.
Homopolymerization PP in the present embodiment is the S2040 of Shanghai match section, is copolymerized the K9829H that PP is sinopec, nitrogen phosphorus fire retardant
For the QB-B01 of neat rich chemical industry.
Embodiment 1
HOPP:33.6%, COPP:35%, antimony oxide:7%, nitrogen phosphorus fire retardant:22%, antioxygen
Agent 168:1.4%, calcium stearate:1.0%;
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 2
HOPP:36.6%, COPP:32%, antimony oxide:7%, nitrogen phosphorus fire retardant:22%, antioxygen
Agent 168:1.4%, calcium stearate:1.0%;
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 3
HOPP:36%, COPP:32%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, antioxygen
Agent 168:1.4%, calcium stearate:1.0%;
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 4
HOPP:36%, COPP:32%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, antioxygen
Agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 5
HOPP:36%, COPP:32%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, antioxygen
Agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Wherein, the preparation side of cyclodextrin cladding antimony oxide
Method is:It is 1 according to the mol ratio of cyclodextrin and antimony oxide:1 weighs each raw material, and cyclodextrin is scattered in absolute ethyl alcohol,
4000r/min stirs 30min, then heats to 80 DEG C, adds antimony oxide, is persistently stirred with 500r/min, insulation reaction
4h, after centrifugal filtration, absolute ethyl alcohol washing, it is put in 60 DEG C of vacuum drying chamber and dries, obtains cyclodextrin cladding antimony oxide.
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 6
HOPP:36%, COPP:32%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, antioxygen
Agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Wherein, the preparation side of cyclodextrin cladding antimony oxide
Method is:It is 1.5 according to the mol ratio of cyclodextrin and antimony oxide:1 weighs each raw material, and cyclodextrin is scattered in into absolute ethyl alcohol
In, 4000r/min stirring 30min, 80 DEG C are then heated to, antimony oxide is added, is persistently stirred with 500r/min, insulation is anti-
4h is answered, after centrifugal filtration, absolute ethyl alcohol washing, is put in 60 DEG C of vacuum drying chamber and dries, obtains the oxidation two of cyclodextrin cladding three
Antimony.
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 400rmp/ after each component is weighed
4min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 25HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Embodiment 7
HOPP:40%, COPP:33%, antimony oxide:7%, nitrogen phosphorus fire retardant:18%, antioxidant
DLTP:0.4%, irgasfos 168:0.7%, calcium stearate:0.9%;
In terms of 100KG, each component is weighed according to above-mentioned percentage by weight, in rotating speed is 500rmp/ after each component is weighed
5min is mixed in min high speed mixer, is well mixed each component.Above-mentioned compound is added in double screw extruder, squeezed
Go out to be granulated;Wherein, double screw extruder engine speed is 29HZ, and temperature is 210-230 DEG C.To the well mixed sampling of finished product, use
Dumbbell shaped iso standard and 3.2mm flame retardant test battens is made in injection machine, and material is carried out according to mechanical property requirements and anti-flammability
Properties are tested.
Comparative example 1
HOPP:68%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, anti-oxidant DLTP:0.7%, resist
Oxygen agent 168:0.7%, calcium stearate:1.0%;Preparation process is same as Example 4, does not repeat herein.
Comparative example 2
HOPP:28%, COPP:40%, antimony oxide:8%, nitrogen phosphorus fire retardant:21.6%, antioxygen
Agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Preparation process is same as Example 4, does not repeat herein.
Comparative example 3
HOPP:36%, COPP:32%, antimony oxide:10%, nitrogen phosphorus fire retardant:19.6%, resist
Oxygen agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Preparation process is same as Example 4, does not go to live in the household of one's in-laws on getting married herein
State.
Comparative example 4
HOPP:36%, COPP:32%, antimony oxide:5.6%, nitrogen phosphorus fire retardant:24%, antioxygen
Agent DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Preparation process is same as Example 4, does not repeat herein.
Comparative example 5
HOPP:36%, COPP:32%, cyclodextrin and antimony oxide:8%, nitrogen phosphorus fire retardant:
21.6%, anti-oxidant DLTP:0.7%, irgasfos 168:0.7%, calcium stearate:1.0%;Wherein, according to cyclodextrin and three oxygen
The mol ratio for changing two antimony is 1.8:1 carries out physical mixed.Preparation process is same as Example 4, does not repeat herein.
Embodiment 1-7 and comparative example 1-5 detection performance result is as shown in table 1.
The embodiment 1-7 of table 1 and comparative example 1-5 performance value
Using cyclodextrin parcel antimony oxide, wherein embodiment 6 is optimal reality of the invention for embodiment 5 and embodiment 6
Example is applied, performance parameter is best, and comparative example 5 is that cyclodextrin mixes with the simple physical of antimony oxide, and this hybrid mode is to material
Expect the no any help of lifting of performance.The proportioning of the present invention, its fire resistance and power is not used in comparative example 1-4 experimental program
Learning performance has different degrees of reduction with respect to embodiment 1-7.
It is in addition, right in place of the non-limit of claimed technical scope midrange and in embodiment technical scheme
The new technical scheme that the equal replacement of single or multiple technical characteristics is formed, equally all in claimed model
In enclosing;Simultaneously the present invention program it is all enumerate or unrequited embodiment in, parameters in the same embodiment are only
Represent an example (i.e. a kind of feasible scheme) for its technical scheme.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be substituted using similar mode, but simultaneously
Do not deviate by the spirit of the present invention or surmount scope defined in appended claims.
Claims (10)
1. a kind of halogen-free anti-flaming polypropylene material, it is characterised in that the halogen-free anti-flaming polypropylene material includes following weight hundred
Divide the component of ratio:
HOPP:32.4~45.4%,
COPP:30~35%,
Antimony oxide:7~8%,
Nitrogen phosphorus fire retardant:16~22%,
Antioxidant:0.8~1.6%,
Processing aid:0.8~1.0%.
A kind of 2. halogen-free anti-flaming polypropylene material according to claim 1, it is characterised in that the HOPP and altogether
It is (1.1-1.5) to gather polyacrylic weight ratio:1.
3. a kind of halogen-free anti-flaming polypropylene material according to claim 1, it is characterised in that the nitrogen phosphorus fire retardant and three
The weight ratio for aoxidizing two antimony is (2.2-2.8):1.
A kind of 4. halogen-free anti-flaming polypropylene material according to claim 1 or 3, it is characterised in that the antimony oxide
Antimony oxide is wrapped up for cyclodextrin.
5. a kind of halogen-free anti-flaming polypropylene material according to claim 4, it is characterised in that the cyclodextrin wraps up three oxygen
The preparation method for changing two antimony is:Cyclodextrin is scattered in ethanol, 3000~5000r/min stirs 20~40min, then heats up
To 80~100 DEG C, antimony oxide is added, 300~500r/min is persistently stirred, 3~5h of insulation reaction, filtering, washing, is done
It is dry.
6. a kind of halogen-free anti-flaming polypropylene material according to claim 5, it is characterised in that the cyclodextrin and three oxidations
The mol ratio of two antimony is (1.2-1.5):1.
7. a kind of halogen-free anti-flaming polypropylene material according to claim 1, it is characterised in that the antioxidant is antioxidant
1010th, the one or more in antioxidant 1076, antioxidant 1135, antioxidant 1098, irgasfos 168, anti-oxidant DLTP.
8. a kind of halogen-free anti-flaming polypropylene material according to claim 1, it is characterised in that the processing aid is PE
One or more in wax, ethylene bis stearamide (EBS), calcium stearate, silicone.
A kind of 9. preparation method of halogen-free anti-flaming polypropylene material as claimed in claim 1, it is characterised in that the preparation method
Including:Each component is weighed according to percentage by weight, after being well mixed, is added in double screw extruder, extruding pelletization;Wherein, it is double
Screw extruder engine speed 25-31HZ, temperature are 210-230 DEG C.
A kind of 10. application of the halogen-free anti-flaming polypropylene material as claimed in claim 1 in the Plastic Drum for accommodating combustible material.
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