CN113388198A - Halogen-free flame-retardant polypropylene composite material and preparation method thereof - Google Patents
Halogen-free flame-retardant polypropylene composite material and preparation method thereof Download PDFInfo
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- CN113388198A CN113388198A CN202110637894.5A CN202110637894A CN113388198A CN 113388198 A CN113388198 A CN 113388198A CN 202110637894 A CN202110637894 A CN 202110637894A CN 113388198 A CN113388198 A CN 113388198A
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- graphene oxide
- composite material
- halogen
- flame retardant
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 62
- -1 polypropylene Polymers 0.000 title claims abstract description 62
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 62
- 239000003063 flame retardant Substances 0.000 title claims abstract description 57
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 48
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 10
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical group [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
- 239000002341 toxic gas Substances 0.000 abstract description 4
- 230000005496 eutectics Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- C08L2201/14—Gas barrier composition
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention discloses a preparation method of a halogen-free flame-retardant polypropylene composite material, which comprises the following components in parts by weight: 60-70 parts of polypropylene, 10-20 parts of edge graphene oxide modified master batch, 10-15 parts of compound flame retardant, 1-2 parts of antioxidant and 2-4 parts of processing agent, and the preparation method comprises the steps of mixing the raw materials in proportion and then carrying out eutectic melting. According to the invention, the edge graphene oxide can effectively prevent the overflow of combustible or toxic gas formed by polymer decomposition and the entrance of external heat and oxygen, so that the flame retardant efficiency is high, and the mechanical property is improved.
Description
Technical Field
The invention relates to a composite material and preparation, in particular to a halogen-free flame-retardant polypropylene composite material and a preparation method thereof.
Background
Polypropylene is a general thermoplastic and is widely applied in the fields of automobile industry, electrical appliance industry, daily necessities, packaging industry and the like. However, polypropylene has a large shrinkage rate, is easily scratched and aged on the surface, is easily burnt when encountering fire, and drops with flame in the burning process and releases a large amount of black smoke, so that the application of polypropylene materials is limited, and the application field of polypropylene needs to be expanded by modifying. As the safety consciousness and the environmental protection consciousness of people are enhanced, the requirement on the environment-friendly flame-retardant polypropylene is increased. The traditional bromine system has high flame retardant efficiency, but because the bromine system is a gas phase flame retardant mechanism, the oxygen index is not high, the smoke density is high during combustion, and a large amount of toxic hydrogen halide gas is released. And the common intumescent flame retardant and hydroxide flame retardant have low flame retardant efficiency and large addition amount, and simultaneously reduce the mechanical property of the composite material.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a halogen-free flame-retardant polypropylene composite material and a preparation method thereof, and solves the problems that the existing polypropylene composite material releases toxic gas during combustion, has low flame-retardant efficiency and influences mechanical properties.
The technical scheme is as follows: the halogen-free flame-retardant polypropylene composite material comprises the following components in parts by weight:
60-70 parts of polypropylene, 10-20 parts of edge graphene oxide modified master batch, 10-15 parts of compound flame retardant, 1-2 parts of antioxidant and 2-4 parts of processing agent.
The composite flame retardant is a nitrogen-phosphorus composite flame retardant with the particle size of 3-6 microns.
In order to uniformly mix the modified master batch with polypropylene at the later stage, the edge graphene oxide modified master batch is prepared from the following raw materials in a weight ratio of 1: 5-1: 20, the edge graphene oxide and the polypropylene matrix are mixed and dissolved.
The preparation method of the halogen-free flame-retardant polypropylene composite material is characterized by comprising the following steps of:
(1) preparing edge graphene oxide modified master batch;
(2) and mixing the prepared edge graphene oxide modified master batch with other raw materials according to the component proportion, and carrying out melt blending to obtain the halogen-free flame-retardant polypropylene composite material.
In the step (1), the edge graphene oxide and the polypropylene matrix are added into a granulator according to a proportion for granulation, and the temperature of the granulator barrel of the granulator is as follows: the first region 158-.
In order to make the mixing more uniform, the step (2) is carried out the melt blending in a twin-screw extruder, the screw rotation speed is 30-50r/min, and the temperature in the barrel of the extruder is set as one region 158-.
The technical principle is as follows: according to the invention, the edge graphene oxide can effectively prevent the overflow of combustible or toxic gas formed by polymer decomposition and the entrance of external heat and oxygen, and in a microscopic view, the edge graphene oxide lamellar structure is overall dense and continuous, and can prevent oxygen from entering the deep part of the material, and the dense and continuous structure has a larger specific surface area in a macroscopic view, and the extremely high specific surface area is easier to adsorb organic volatile matters generated in the combustion process and prevent the organic volatile matters from being released and diffused in the combustion process. In addition, oxygen radicals on the edges are decomposed and dehydrated at low temperature, so that the pyrolysis temperature is reduced, oxygen supply is diluted, a carbon layer generated by a decomposition product of the polymer is compact due to the synergistic effect of the edge graphene oxide and the compound flame retardant, the strength of a carbon layer framework is higher, and the mechanical strength is favorably improved.
Has the advantages that: according to the invention, the edge graphene oxide is adopted to modify the polypropylene, the large specific surface area of the edge graphene oxide can effectively prevent the overflow of combustible or toxic gas formed by the decomposition of the polymer, and the synergistic effect of the edge graphene oxide and the nitrogen-phosphorus compound flame retardant can not only improve the flame retardant efficiency of the polypropylene, but also improve the mechanical property of the polypropylene.
Detailed Description
The present invention is further explained below.
Example 1
The halogen-free flame-retardant polypropylene composite material comprises 60 parts by weight of a polypropylene matrix, 10 parts by weight of edge graphene oxide modified master batches, 10 parts by weight of a compound flame retardant, 1 part by weight of an antioxidant and 2 parts by weight of a processing agent; the edge graphene oxide modified master batch is prepared from the following components in parts by weight of 1: 5, the edge graphene oxide and the polypropylene matrix are mixed and melted.
During preparation, the raw materials are weighed according to the proportion, the edge graphene oxide modified master batch is prepared, and finally the edge graphene oxide modified master batch, the polypropylene matrix and other raw materials are subjected to melt blending according to the proportion to obtain the product. The method is characterized in that the edge graphene oxide and the polypropylene matrix are added into a granulator according to the proportion for granulation, and the temperature of the granulator barrel of the granulator is as follows: : the first zone is 165 ℃, the second zone is 170 ℃, the third zone is 175 ℃, the fourth zone is 181 ℃, and the temperature of the die is 192 ℃. Adding the polypropylene matrix, the edge graphene oxide modified master batch, the compound flame retardant, the antioxidant and the processing agent into a mixer, mixing for 1h, adding the uniformly mixed materials into a double-screw extruder, wherein the screw rotating speed is 40r/min, the temperature in the barrel of the extruder is set to be 158 ℃ in the first zone, 168 ℃ in the second zone, 175 ℃ in the third zone and 181 ℃ in the fourth zone, and extruding the mixture through the extruder to obtain the high-performance flame-retardant polypropylene composite material.
Example 2
The halogen-free flame-retardant polypropylene composite material comprises a polypropylene matrix, edge graphene oxide modified master batches, a compound flame retardant, an antioxidant and a processing agent, wherein the polypropylene matrix comprises 65 parts by weight, the edge graphene oxide modified master batches comprise 15 parts by weight, the compound flame retardant comprises 13 parts by weight, the antioxidant comprises 2 parts by weight and the processing agent comprises 2 parts by weight; the edge graphene oxide modified master batch is prepared from the following raw materials in parts by weight of 1: 10, the edge graphene oxide and the polypropylene matrix are mixed and melted.
During preparation, the raw materials are weighed according to the proportion, the edge graphene oxide modified master batch is prepared, and finally the edge graphene oxide modified master batch, the polypropylene matrix and other raw materials are subjected to melt blending according to the proportion to obtain the product. The method is characterized in that the edge graphene oxide and the polypropylene matrix are added into a granulator according to the proportion for granulation, and the temperature of the granulator barrel is as follows: : the first zone is 158 ℃, the second zone is 174 ℃, the third zone is 180 ℃, the fourth zone is 185 ℃, and the temperature of the die is 192 ℃. Adding the polypropylene matrix, the edge graphene oxide modified master batch, the compound flame retardant, the antioxidant and the processing agent into a mixer, mixing for 1h, adding the uniformly mixed mixture into a double-screw extruder, wherein the screw rotation speed is 35r/min, the temperature in the barrel of the extruder is set to be 160 ℃ in the first zone, 170 ℃ in the second zone, 178 ℃ in the third zone and 184 ℃ in the fourth zone, and extruding the mixture through the extruder to obtain the high-performance flame-retardant polypropylene composite material.
Example 3
The halogen-free flame-retardant polypropylene composite material comprises 70 parts of a polypropylene matrix, 20 parts of edge graphene oxide modified master batches, 15 parts of a compound flame retardant, 2 parts of an antioxidant and 3 parts of a processing agent according to the weight ratio; the edge graphene oxide modified master batch is prepared from the following components in parts by weight of 1: 15, the edge graphene oxide and the polypropylene matrix are mixed and melted.
During preparation, the raw materials are weighed according to the proportion, the edge graphene oxide modified master batch is prepared, and finally the edge graphene oxide modified master batch, the polypropylene matrix and other raw materials are subjected to melt blending according to the proportion to obtain the product. The method is characterized in that the edge graphene oxide and the polypropylene matrix are added into a granulator according to the proportion for granulation, and the temperature of the granulator barrel is as follows: : the first zone was 168 ℃, the second zone was 173 ℃, the third zone was 179 ℃, the fourth zone was 182 ℃, and the mold temperature was 192 ℃. And adding the polypropylene matrix, the edge graphene oxide modified master batch, the compound flame retardant, the antioxidant and the processing agent into a mixer, mixing for 1h, adding the uniformly mixed mixture into a double-screw extruder, wherein the screw rotation speed is 50r/min, the temperature in the barrel of the extruder is set to be 158 ℃ in the first zone, 169 ℃ in the second zone, 176 ℃ in the third zone and 185 ℃ in the fourth zone, and extruding the mixture through the extruder to obtain the high-performance flame-retardant polypropylene composite material.
Preparing three high-performance halogen-free flame-retardant polypropylene composite material samples with the same size and specification respectively according to the methods of the embodiments 1 to 3, and recording the three samples as a sample 1, a sample 2 and a sample 3, then preparing a comparative sample with the same size and specification as the sample 1 by adopting the method of the invention, and recording the comparative sample as a sample 4, wherein the difference between the sample 4 and the sample 1 is that edge graphene oxide is not added; sample 5 was prepared according to the method of the present invention and the weight ratio of the starting materials in sample 5 was identical to that of sample 2, with the difference that: the edge graphene oxide is not mixed with the polypropylene matrix to prepare edge graphene oxide modified master batch, but is directly mixed with other materials uniformly and then extruded to prepare the final product.
The mechanical strength and the flame retardant property of the samples are respectively measured under the same conditions, and the test results are as follows:
as can be seen from the above table, compared with comparative sample 4, the halogen-free polypropylene composite material of the present invention has excellent flame retardant properties such as high oxygen index, flame retardant V-0, etc., and simultaneously has good mechanical properties. It can be seen from comparing samples 1, 2 and 3 that when the content of the flame retardant is too high or too low, both the flame retardant property and the mechanical property of the polypropylene are affected, and when the content of the flame retardant is higher, the dispersion is not uniform in the polypropylene, thereby lowering the tensile strength and the limiting oxygen index. When comparing samples 2 and 5, it is found that the edge graphene oxide and the polypropylene matrix are mixed and dissolved to prepare the edge graphene oxide modified master batch, which is more beneficial to uniformly mixing the polypropylene and the flame retardant, so that the performance of the polypropylene is improved. Therefore, the edge graphene oxide and the nitrogen-phosphorus compound flame retardant in the flame-retardant composite material have the effects of mutual promotion and mutual synergy, and can play a significant flame-retardant effect and improve the mechanical property.
Claims (6)
1. The halogen-free flame-retardant polypropylene composite material is characterized by comprising the following components in parts by weight:
60-70 parts of polypropylene, 10-20 parts of edge graphene oxide modified master batch, 10-15 parts of compound flame retardant, 1-2 parts of antioxidant and 2-4 parts of processing agent.
2. The halogen-free flame retardant polypropylene composite material according to claim 1, wherein the compound flame retardant is a nitrogen-phosphorus compound flame retardant, and the particle size is 3-6 microns.
3. The halogen-free flame-retardant polypropylene composite material according to claim 1, wherein the edge graphene oxide modified master batch is prepared from the following raw materials in a weight ratio of 1: 5-1: 20, the edge graphene oxide and the polypropylene matrix are mixed and melted.
4. The preparation method of the halogen-free flame retardant polypropylene composite material according to claim 1, comprising the following steps:
(1) preparing edge graphene oxide modified master batch;
(2) and mixing the prepared edge graphene oxide modified master batch with other raw materials according to the component proportion, and carrying out melt blending to obtain the halogen-free flame-retardant polypropylene composite material.
5. The preparation method of the halogen-free flame retardant polypropylene composite material according to claim 4, wherein in the step (1), the edge graphene oxide and the polypropylene matrix are proportionally added into a granulator for granulation, and the temperature of the barrel of the granulator is as follows: the first region 158-.
6. The method for preparing the halogen-free flame retardant polypropylene composite material as claimed in claim 4, wherein the step (2) comprises melt blending in a twin-screw extruder at a screw rotation speed of 30-50r/min, wherein the temperatures in the barrel of the extruder are set to be 158 ℃ in one zone, 168 ℃ in two zones, 175 ℃ in three zones and 181 ℃ in three zones and 186 ℃ in four zones and 181 ℃ in 186 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110637894.5A CN113388198A (en) | 2021-06-08 | 2021-06-08 | Halogen-free flame-retardant polypropylene composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110637894.5A CN113388198A (en) | 2021-06-08 | 2021-06-08 | Halogen-free flame-retardant polypropylene composite material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN113388198A true CN113388198A (en) | 2021-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110637894.5A Pending CN113388198A (en) | 2021-06-08 | 2021-06-08 | Halogen-free flame-retardant polypropylene composite material and preparation method thereof |
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| CN (1) | CN113388198A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115651307A (en) * | 2022-09-07 | 2023-01-31 | 深圳力越新材料有限公司 | Polypropylene composite material and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN108467547A (en) * | 2018-04-04 | 2018-08-31 | 宁波福天新材料科技有限公司 | A kind of converter environment-protection flame-proof electrostatic resistance polypropylene composition and preparation method thereof |
| CN109179393A (en) * | 2018-11-05 | 2019-01-11 | 盐城师范学院 | A kind of preparation method of limbic function graphite alkene |
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2021
- 2021-06-08 CN CN202110637894.5A patent/CN113388198A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467547A (en) * | 2018-04-04 | 2018-08-31 | 宁波福天新材料科技有限公司 | A kind of converter environment-protection flame-proof electrostatic resistance polypropylene composition and preparation method thereof |
| CN109179393A (en) * | 2018-11-05 | 2019-01-11 | 盐城师范学院 | A kind of preparation method of limbic function graphite alkene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651307A (en) * | 2022-09-07 | 2023-01-31 | 深圳力越新材料有限公司 | Polypropylene composite material and preparation method thereof |
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Application publication date: 20210914 |