CN107254106A - A kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material and preparation method thereof - Google Patents
A kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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- CN107254106A CN107254106A CN201710386260.0A CN201710386260A CN107254106A CN 107254106 A CN107254106 A CN 107254106A CN 201710386260 A CN201710386260 A CN 201710386260A CN 107254106 A CN107254106 A CN 107254106A
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- 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
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Abstract
The present invention provides a kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material and preparation method thereof, is related to technical field of polymer materials.Stratiform hypophosphites flame-proof reinforced polypropylene composite material of the present invention is made up of following raw material：Acrylic resin, stratiform hypophosphites, toughener, antioxidant, light stabilizer, lubricant.The present invention first synthesizes stratiform hypophosphites using hydro-thermal method, stratiform hypophosphites nanometer sheet is well combined with polypropylene matrix, be evenly distributed in polypropylene matrix, good dispersion, small is influenceed on the mechanical property of materials, the PP composite material intensity for adding its preparation is high, heat endurance is good.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of stratiform hypophosphites flame-proof reinforced polypropylene is answered
Condensation material and preparation method thereof.
Background technology
Hypophosphites is excellent performance and a kind of environment amenable nontoxic fire retardant of Halogen.It has phosphorus content high
(41.89%), heat endurance is good and the advantages of excellent fireproof performance.High polymer material is applied to as a kind of new fire retardant
In, receive very good effect.The hypo-aluminum orthophosphate for utilizing Co deposited synthesis is used for polystyrene (PS) by Wang Yuzhong etc.
In fire-retardant, as a result showing the hypo-aluminum orthophosphate of 25 parts of addition can make composite reach UL-94V0 ranks, while limited oxygen index
33.3% is reached, the fire resistance of PS composites can be effectively improved, HRR is reduced.
In the prior art, commercially available hypophosphites is prepared using coprecipitation mostly, with particle diameter is larger, pattern is each
Different, skewness and the dispersed defect such as poor in the material, cause the flame retarding efficiency of PP composite material low, and right
The Effect on Mechanical Properties of PP composite material is larger so that PP composite material low intensity, heat endurance are poor.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide a kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material and its
Preparation method, solving hypophosphites particle diameter in the prior art, greatly, skewness, bad dispersibility, add its preparation in the material
PP composite material low intensity, heat endurance is poor, poor fire technical problem.
To realize object above, technical scheme is achieved by the following technical programs：
A kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material, layered hypophosphites flame-proof reinforced polypropylene
Composite is made up of the raw material of following parts by weight：60-80 parts of acrylic resin, 10-15 parts of stratiform hypophosphites, toughener 5-
15 parts, 0.3-0.5 parts of antioxidant, 0.2-0.4 parts of light stabilizer, 0.3-0.5 parts of lubricant.
It is preferred that, the acrylic resin is at least one of COPP, HOPP.
It is preferred that, layered hypophosphites is the nanometer sheet synthesized through hydro-thermal method.
It is preferred that, layered hypophosphites be stratiform hypo-aluminum orthophosphate, stratiform magnesium hypophosphite, stratiform ferric hypophosphite in extremely
Few one kind.
It is preferred that, the preparation method of layered hypophosphites is：By weight 1：2-2.3：0.01-0.05 weighs metal
Salt, sodium hypophosphite and surfactant, are placed in autoclave, using absolute ethyl alcohol as solvent, stirring, after being completely dissolved, in 230 DEG C
Baking oven in handle 3h, suction filtration after being washed successively with water, ethanol, is placed in vacuum drying oven and dried, stratiform hypophosphorous acid is made in grinding
Salt.
It is preferred that, the metal salt be aluminium chloride, aluminum sulfate, magnesium chloride, magnesium sulfate, iron chloride and ferric sulfate at least
It is a kind of.
It is preferred that, the surfactant is fatty glyceride, polyalcohol, polyoxyethylene-type, polyoxyethylene-polyoxy third
At least one of alkene copolymer.
It is preferred that, the toughener is in ethylene-propylene copolymer, ethylene-butene copolymer, ethylene-octene copolymer
At least one, the antioxidant is Hinered phenols antioxidant, aromatic amine kind antioxidant, phosphite ester kind antioxidant, thio
At least one of dipropyl acid diester, the light stabilizer is salicylic acid lipid light stabilizer, benzophenone light stabilizer, benzene
At least one of and triazole type light stabilizer, the lubricant is selected from hydrocarbon lubricants, fatty acid acyl amine and its derivative
At least one of.
It is preferred that, the thickness of the nanometer sheet is 500nm, and length is 20um, and width is 4um.
A kind of preparation method of stratiform hypophosphites flame-proof reinforced polypropylene composite material, comprises the following steps：
S1, by 1：2.0-2.3：0.01-0.05 weight ratio weighs metal salt, sodium hypophosphite and surfactant, is placed in
In autoclave, using absolute ethyl alcohol as solvent, stirring after being completely dissolved, handles 3h, suction filtration is used successively in 230 DEG C of baking oven
After water, ethanol washing, it is placed in vacuum drying oven and dries, stratiform hypophosphites is made in grinding；
S2, the acrylic resin of parts by weight, toughener, antioxidant, light stabilizer and lubricant be added to high-speed stirred
3-5min is mixed in machine, mixed material is obtained；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by step S1
Stratiform hypophosphites added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dry obtained stratiform hypophosphites and hinder
Fire reinforced polypropylene compound material；Wherein, twin-screw extruder barrel temperature is 190-220 DEG C, and screw speed is 400-500r/
Min, engine speed is 18-22Hz, and vacuum is -0.06-0.08MPa.
The present invention provides a kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material and preparation method thereof, with existing skill
Art is compared to advantage：
Stratiform hypophosphites in stratiform hypophosphites flame-proof reinforced polypropylene composite material raw material of the present invention is to utilize water
The stratiform hypophosphites nanometer sheet of hot method synthesis, the unique laminated structure of stratiform hypophosphites nanometer sheet rises in pressurized process
Bridging action is arrived, making the bending strength of PP composite material increases, while it has larger specific surface area, can be more effective
Ground promotes PP composite material into charcoal process, makes the layer of charcoal to be formed more dense uniform, the radiation of barrier outside heat and oxygen
The entrance of gas, so as to greatly improve the fire resistance of PP composite material；The stratiform hypophosphites of hydro-thermal method synthesis simultaneously is received
Rice piece, surface property is improved so that stratiform hypophosphites nanometer sheet powder is well combined with polypropylene matrix, in polypropylene
Be evenly distributed in matrix, good dispersion, on the mechanical property of materials influence it is small, add its preparation PP composite material intensity
High, heat endurance is good；
The stratiform hypophosphites used in the present invention, the raw material of synthesis are easy to buying, economical, environmentally friendly, efficient, subsequently should
With quite varied, production cost is reduced.
In the preparation method of stratiform hypophosphites disclosed by the invention, using the relatively low dielectric constant of ethanol, it is certain also
Originality, prepares the homogeneous stratiform hypophosphites nanometer sheet of pattern, and contain reactive function by the method for Hydrothermal Synthesiss
The compatibility of group's (light base, carboxyl etc.), increase hypophosphites and polymer, it is small to the Effect on Mechanical Properties of material, its uniqueness
Laminated structure, serves bridging action in pressurized process, makes the bending strength of composite and increases.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, with reference to the embodiment of the present invention pair
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is a part of the invention
Embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making wound
The every other embodiment obtained under the premise of the property made work, belongs to the scope of protection of the invention.
Herein using the relatively low dielectric constant of ethanol, certain reproducibility, pattern is prepared by the method for Hydrothermal Synthesiss
Homogeneous hypophosphites nanometer sheet, and contain reactive functional group (light base, carboxyl etc.), increase hypophosphites and polymer
Compatibility, its unique laminated structure small to the Effect on Mechanical Properties of material serve bridging action in pressurized process,
Making the bending strength of composite increases.It has larger specific surface area simultaneously, can more effectively promote composite into charcoal
Process, makes the layer of charcoal to be formed more dense uniform, the radiation and the entrance of oxygen of barrier outside heat, so as to greatly improve
The fire resistance of composite.
Embodiment 1：
The present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
The preparation method of the present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material, comprises the following steps：
S1,100g aluminium chloride, 200g sodium hypophosphites, 1gPVP be placed in autoclave, using absolute ethyl alcohol as solvent, stirring,
After being completely dissolved, 3h is handled in 230 DEG C of baking oven, suction filtration after being washed respectively with water, ethanol, is placed in vacuum drying oven and dried,
Stratiform hypo-aluminum orthophosphate is made in grinding；
S2,75 parts of acrylic resin copolymer, 10 parts of toughener POE5070D, 0.3 part of antioxidant 1010,0.2 part resisted
Oxygen agent 168,0.2 part of light stabilizer 5585 and 0.3 part of lubricant silicone powder are added in homogenizer mix 5min together,
Obtain mixed material；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by 15 parts of steps
Stratiform hypo-aluminum orthophosphate in S1 is added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dries obtained low-odor polypropylene
Alkene composite；Wherein, extruder barrel temperature be 190 DEG C, screw speed be that 400r/min, engine speed are 18Hz, vacuum
Spend for -0.06MPa.
Embodiment 2：
The present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
The preparation method of the present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material, comprises the following steps：
S1,100g ferric sulfate, 210g sodium hypophosphites, 1gPVP be placed in autoclave, using absolute ethyl alcohol as solvent, stirring,
After being completely dissolved, 3h is handled in 230 DEG C of baking oven, suction filtration after being washed respectively with water, ethanol, is placed in vacuum drying oven and dried,
Stratiform ferric hypophosphite is made in grinding；
S2, by 75 parts of acrylic resin copolymer, 10 parts of toughener POE875L, 0.3 part of antioxidant 1076,0.2 part of antioxygen
Agent 168,0.2 part of light stabilizer V703 and 0.3 part of lubricant TR451 are added in homogenizer mix 5min together, obtain
To mixed material；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by 15 parts of steps
Stratiform hypo-aluminum orthophosphate in S1 is added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dries obtained low-odor polypropylene
Alkene composite；Wherein, extruder barrel temperature be 190 DEG C, screw speed be that 400r/min, engine speed are 18Hz, vacuum
Spend for -0.06MPa.
Embodiment 3：
The present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
The preparation method of the present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material, comprises the following steps：
S1,200g magnesium sulfate, 230g sodium hypophosphites, 5g Pluronic F68s be placed in autoclave, with
Absolute ethyl alcohol is solvent, stirring, after being completely dissolved, 3h is handled in 230 DEG C of baking oven, suction filtration is washed with water, ethanol respectively
Afterwards, it is placed in vacuum drying oven and dries, stratiform magnesium hypophosphite is made in grinding；
S2, by 60 parts of HOPP resins, 5 parts of ethylene-octene copolymers, 0.3 part of antioxidant 1076,0.2 part of antioxygen
Agent 168,0.2 part of benzotriazole light stabilizer and 0.3 part of lubricant TR451 are added in homogenizer and mixed together
5min, obtains mixed material；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by 10 parts of steps
Stratiform hypo-aluminum orthophosphate in S1 is added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dries obtained low-odor polypropylene
Alkene composite；Wherein, extruder barrel temperature be 220 DEG C, screw speed be that 500r/min, engine speed are 22Hz, vacuum
Spend for 0.08MPa.
Embodiment 4：
The present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
The preparation method of the present embodiment stratiform hypophosphites flame-proof reinforced polypropylene composite material, comprises the following steps：
S1,100g ferric sulfate, 210g sodium hypophosphites, 1gPVP be placed in autoclave, using absolute ethyl alcohol as solvent, stirring,
After being completely dissolved, 3h is handled in 230 DEG C of baking oven, suction filtration after being washed respectively with water, ethanol, is placed in vacuum drying oven and dried,
Stratiform ferric hypophosphite is made in grinding；
S2, by 80 parts of acrylic resin copolymer, 15 parts of toughener POE875L, 0.2 part of antioxidant 1076,0.1 part of antioxygen
Agent 168,0.4 part of light stabilizer V703 and 0.5 part of lubricant TR451 are added in homogenizer mix 5min together, obtain
To mixed material；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by 12 parts of steps
Stratiform hypo-aluminum orthophosphate in S1 is added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dries obtained low-odor polypropylene
Alkene composite；Wherein, extruder barrel temperature be 200 DEG C, screw speed be that 450r/min, engine speed are 20Hz, vacuum
Spend for 0.02MPa.
Comparative example 1：
This comparative example stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
Specific preparation method comprises the following steps：
S1,75 parts of acrylic resin copolymer, 10 parts of toughener POE5070D, 0.3 part of antioxidant 1010,0.2 part resisted
Oxygen agent 168,0.2 part of light stabilizer 5585 and 0.3 part of lubricant silicone powder are added in homogenizer mix 5min together,
Obtain mixed material；
S2, by the material in step S1 by main feeding hopper add double screw extruder in, by 15 parts of commercially available secondary phosphorus
Sour aluminium is added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dries obtained low odor polypropylene composite material；Its
In, extruder barrel temperature is 190 DEG C, screw speed is that 400r/min, engine speed are 18Hz, and vacuum is -0.06MPa.
Comparative example 2：
This comparative example stratiform hypophosphites flame-proof reinforced polypropylene composite material is made up of the raw material of following parts by weight：
Specific preparation method comprises the following steps：
S1, by 75 parts of acrylic resin copolymer, 10 parts of toughener POE875L, 0.3 part of antioxidant 1076,0.2 part of antioxygen
Agent 168,0.2 part of light stabilizer V703 and 0.3 part of lubricant TR451 are added in homogenizer mix 5min together, obtain
To mixed material；
S2, by the material in step S1 by main feeding hopper add double screw extruder in, by 15 parts of commercially available ferric hypophosphites
Added by the natural exhaust outlet side of first paragraph, through melting, extrusion, dry obtained low odor polypropylene composite material；Wherein, squeeze
Go out machine barrel temperature be 190 DEG C, screw speed be that 400r/min, engine speed are 18Hz, vacuum is -0.06MPa.
By stratiform hypophosphites flame-proof reinforced polypropylene composite material made from above-described embodiment 1,2 and comparative example 1,2
Main physical index according to coherent detection standard testing, its tensile strength, bending strength, bending modulus, impact strength, smell its
Examination criteria is as shown in table 1 with testing result：
The embodiment 1-2 of table 1 and the main physical property of comparative example 1-2 laminate hypophosphites flame-proof reinforced polypropylene composite materials refer to
Mark
The individual material properties test case of table 1
In summary, stratiform hypophosphites is synthesized using hydro-thermal method in the present invention, improves the surface property of powder so that powder
End is well combined with polypropylene matrix, and impact and tensile property influence small；The modified layered hypophosphites used in the present invention, its
Unique laminated structure, serves bridging action, making the bending strength of composite increases in pressurized process.It has simultaneously
Larger specific surface area, can more effectively promote composite into charcoal process, make the layer of charcoal to be formed more dense uniform, and barrier is outer
The radiation of face heat and the entrance of oxygen, HRR are obviously reduced, so as to greatly improve the fire resistance of composite.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although ginseng
The present invention is described in detail according to previous embodiment, it will be understood by those within the art that：It still can be with
Technical scheme described in foregoing embodiments is modified, or equivalent substitution is carried out to which part technical characteristic；And
These modifications are replaced, and the essence of appropriate technical solution is departed from the spirit and model of various embodiments of the present invention technical scheme
Enclose.
Claims (10)
1. a kind of stratiform hypophosphites flame-proof reinforced polypropylene composite material, it is characterised in that layered hypophosphites is fire-retardant
Reinforced polypropylene compound material is made up of the raw material of following parts by weight：60-80 parts of acrylic resin, stratiform hypophosphites 10-15
Part, 5-15 parts of toughener, 0.3-0.5 parts of antioxidant, 0.2-0.4 parts of light stabilizer, 0.3-0.5 parts of lubricant.
2. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1, it is characterised in that：It is described poly-
Allyl resin is at least one of COPP, HOPP.
3. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1, it is characterised in that：The layer
Shape hypophosphites is the nanometer sheet synthesized through hydro-thermal method.
4. the stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1 or 3, it is characterised in that：Institute
It is at least one of stratiform hypo-aluminum orthophosphate, stratiform magnesium hypophosphite, stratiform ferric hypophosphite to state stratiform hypophosphites.
5. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1, it is characterised in that the layer
The preparation method of shape hypophosphites is：By weight 1：2-2.3：0.01-0.05 weighs metal salt, sodium hypophosphite and surface-active
Agent, is placed in autoclave, using absolute ethyl alcohol as solvent, stirring, after being completely dissolved, handles 3h in 230 DEG C of baking oven, suction filtration,
After being washed successively with water, ethanol, it is placed in vacuum drying oven and dries, stratiform hypophosphites is made in grinding.
6. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 5, it is characterised in that：The gold
Category salt is at least one of aluminium chloride, aluminum sulfate, magnesium chloride, magnesium sulfate, iron chloride and ferric sulfate, and the surfactant is
At least one of fatty glyceride, polyalcohol, polyoxyethylene-type, Pluronic F68.
7. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1, it is characterised in that：It is described to increase
Tough dose is at least one of ethylene-propylene copolymer, ethylene-butene copolymer, ethylene-octene copolymer, the antioxidant
For at least one in Hinered phenols antioxidant, aromatic amine kind antioxidant, phosphite ester kind antioxidant, thio-2 acid dibasic acid esters
Kind.
8. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 1, it is characterised in that：The light
Stabilizer is at least one of salicylic acid lipid light stabilizer, benzophenone light stabilizer, benzotriazole light stabilizer,
The lubricant is selected from least one of hydrocarbon lubricants, fatty acid acyl amine and its derivative.
9. stratiform hypophosphites flame-proof reinforced polypropylene composite material according to claim 3, it is characterised in that：It is described to receive
The thickness of rice piece is 500nm, and length is 20um, and width is 4um.
10. it is a kind of such as the preparation side of any layered hypophosphites flame-proof reinforced polypropylene composite material in claim 1-9
Method, it is characterised in that comprise the following steps：
S1, by 1：2.0-2.3：0.01-0.05 weight ratio weighs metal salt, sodium hypophosphite and surfactant, is placed in high pressure
In kettle, using absolute ethyl alcohol as solvent, stirring after being completely dissolved, handles 3h, suction filtration, successively with water, second in 230 DEG C of baking oven
After alcohol washing, it is placed in vacuum drying oven and dries, stratiform hypophosphites is made in grinding；
S2, the acrylic resin of parts by weight, toughener, antioxidant, light stabilizer and lubricant be added in homogenizer
3-5min is mixed, mixed material is obtained；
S3, obtained mixed material in step S2 added in double screw extruder by main feeding hopper, by the layer in step S1
Shape hypophosphites through melting, extrusion, dries the fire-retardant increasing of obtained stratiform hypophosphites by the natural exhaust outlet side addition of first paragraph
Strong PP composite material；Wherein, twin-screw extruder barrel temperature is 190-220 DEG C, and screw speed is 400-500r/min,
Engine speed is 18-22Hz, and vacuum is -0.06-0.08MPa.
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| CN107880417A (en) * | 2017-10-19 | 2018-04-06 | 合肥朗胜新材料有限公司 | A kind of EPS composites and preparation method thereof |
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| CN108314388A (en) * | 2018-05-11 | 2018-07-24 | 安徽砼宇特构科技有限公司 | A kind of fibre reinforced concrete material and preparation method thereof |
| CN108997768A (en) * | 2018-09-03 | 2018-12-14 | 合肥久新不锈钢厨具有限公司 | A kind of preparation method of the anti-flaming environment-friendly panel of furniture |
| CN109796683A (en) * | 2018-12-27 | 2019-05-24 | 会通新材料股份有限公司 | A kind of dialkyl hypophosphorous acid root intercalated houghite enhancing flame-retardant polypropylene composite material and preparation method thereof |
| CN110894337A (en) * | 2019-10-30 | 2020-03-20 | 铜陵昌满塑胶有限公司 | Preparation method of high-performance capacitor shell material |
| CN113278203A (en) * | 2021-06-16 | 2021-08-20 | 山东泰星新材料股份有限公司 | Preparation method and application of efficient halogen-free flame retardant for polypropylene |
| CN116041847A (en) * | 2022-12-28 | 2023-05-02 | 重庆会通科技有限公司 | High-heat-conductivity flame-retardant polypropylene composite material and preparation method thereof |
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| CN104860281A (en) * | 2015-06-01 | 2015-08-26 | 武汉理工大学 | Preparation method of aluminum hypophosphite |
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| CN108314388A (en) * | 2018-05-11 | 2018-07-24 | 安徽砼宇特构科技有限公司 | A kind of fibre reinforced concrete material and preparation method thereof |
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| CN109796683A (en) * | 2018-12-27 | 2019-05-24 | 会通新材料股份有限公司 | A kind of dialkyl hypophosphorous acid root intercalated houghite enhancing flame-retardant polypropylene composite material and preparation method thereof |
| CN110894337A (en) * | 2019-10-30 | 2020-03-20 | 铜陵昌满塑胶有限公司 | Preparation method of high-performance capacitor shell material |
| CN113278203A (en) * | 2021-06-16 | 2021-08-20 | 山东泰星新材料股份有限公司 | Preparation method and application of efficient halogen-free flame retardant for polypropylene |
| CN116041847A (en) * | 2022-12-28 | 2023-05-02 | 重庆会通科技有限公司 | High-heat-conductivity flame-retardant polypropylene composite material and preparation method thereof |
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