CN110790920A - Semi-aromatic polyamide and polyamide molding composition composed of same - Google Patents
Semi-aromatic polyamide and polyamide molding composition composed of same Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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Abstract
The invention discloses a semi-aromatic polyamide which comprises the following repeating units based on the molar content of all repeating units of chain segments: (a) 53 mol/% -71 mol/% of 10T units derived from 1, 10-decanediamine and terephthalic acid; (b) 29mol/% -47 mol% of 10X units derived from 1, 10-decanediamine and at least one of isophthalic acid, 1, 4-cyclohexanedicarboxylic acid, adipic acid, suberic acid, 1, 10-decanedioic acid, 1, 12-dodecanedioic acid, pentadecanedioic acid; wherein, in the semi-aromatic polyamide, the molar content of the bio-based carbon is 39 mol% -100 mol%; in the semi-aromatic polyamide, the amino content is 30-100 mol/ton, and the carboxyl content is 30-200 mol/ton. The invention obtains the semi-aromatic polyamide with excellent colorability by controlling the content of bio-based carbon, the content of amino and carboxyl and the content of each repeating unit of the collocation of monomers.
Description
Technical Field
The invention relates to the technical field of new high-molecular materials, in particular to semi-aromatic polyamide and a molding composition composed of the semi-aromatic polyamide.
Background
The polyamide has good comprehensive properties including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubricity, low friction coefficient, certain flame retardance, easy processing and the like, and is widely suitable for being filled, reinforced and modified by glass fibers and other fillers, so that the performance is improved and the application range is expanded. Semi-aromatic polyamides have been developed in recent years with great emphasis on their superior heat resistance and mechanical properties.
However, the synthetic raw materials of the existing polyamide resins are mainly derived from petroleum cracked products. The petroleum-based polyamide contains some chemically unstable substances, and the substances are easy to generate chemical changes when contacting a high-temperature heat source in the production process, so that the color of the resin is deteriorated and the mechanical properties are lost. Under the conditions of long-time sunshine and long-time heating, the related products are easy to generate phenomena of yellowing, aging and the like, and the appearance and the quality of the products are greatly influenced.
Prior patent application 201710955052.8 discloses that the whiteness of polyamide materials can be increased by increasing the biobased content of the polyamide, with good colour levels. However, this can only improve the color developability by increasing the whiteness of the resin itself, and does not improve the color developability from the degree of binding between the polyamide resin matrix and the pigment. Meanwhile, only improving the whiteness and the anti-yellowing effect of the polyamide cannot obtain a polyamide product with good color.
Factors influencing the coloring property of the bio-based semi-aromatic polyamide are mainly factors such as interaction force between the pigment and the resin and dispersion uniformity of the pigment in the resin matrix. Therefore, the main factor affecting the colorability is the resin matrix itself.
Disclosure of Invention
The purpose of the present invention is to provide a semi-aromatic polyamide having an advantage of good colorability.
It is another object of the present invention to provide a polyamide molding composition comprising the above semi-aromatic polyamide, which can maintain good colorability.
The invention is realized by the following technical scheme:
a semi-aromatic polyamide comprising, based on the molar content of all the recurring units of the chain segment: (a) 53 mol/% -71 mol/% of 10T units derived from 1, 10-decanediamine and terephthalic acid; (b) 29mol/% -47 mol% of 10X units derived from 1, 10-decanediamine and at least one of isophthalic acid, 1, 4-cyclohexanedicarboxylic acid, adipic acid, suberic acid, 1, 10-decanedioic acid, 1, 12-dodecanedioic acid, pentadecanedioic acid; wherein, in the semi-aromatic polyamide, the molar content of the bio-based carbon is 39 mol% -100 mol%; in the semi-aromatic polyamide, the amino content is 30-100 mol/ton, and the carboxyl content is 30-200 mol/ton.
The content of the terminal groups is regulated according to the polymerization method.
The content of the bio-based carbon is measured according to ASTM standard D6866-12/Method-B;
preferably, the repeating unit: (a) 60mol/% -66 mol/% of 10T units; (b) 34 mol/% -40 mol% of 10X units.
Preferably, the 10X units are derived from 1, 10-decanediamine and at least one of 1, 12-dodecanedioic acid, suberic acid.
Preferably, the molar content of the bio-based carbon is 86 mol% to 100 mol%.
Preferably, the semi-aromatic polyamide has an amino group content of 30 to 60 mol/ton and a carboxyl group content of 50 to 80 mol/ton.
The bio-based polyamide contains fewer chemically unstable substances, and the acting force between the pigment and the resin is less influenced; the proper concentration of the end group can also help the pigment enter molecular chains and improve the dispersibility of the pigment. The pigment is easier to disperse in the resin matrix by regulating the content of the bio-based groups, the proportion of the repeating units, the concentration of the end groups and the selection of the monomers, thereby improving the tinting strength of the pigment. Within the preferred range, the coloring property is better.
The bio-based carbon is derived from at least one of 1, 10-decanediamine, terephthalic acid, 1, 10-decanedioic acid, 1, 12-dodecanedioic acid and adipic acid.
The melting point of the semi-aromatic polyamide obtained by the method is 210-300 ℃;
the method for producing the semi-aromatic polyamide in the present invention is not particularly limited. It may be prepared by first subjecting the prepolymer to solid-phase polymerization, or melt-mixing in an extruder. It can also be produced via melt polymerization.
The preparation method comprises the following steps:
adding a reaction monomer, sodium hypophosphite, an antioxidant and deionized water into a reaction kettle according to the proportion, vacuumizing, filling argon as a protective gas, heating to 190-. Heating to 240 ℃ within 3 hours, keeping the temperature for 2 hours, and then opening a valve to discharge to obtain the prepolymer.
Prepolymer in 80oAnd C, performing vacuum drying, and performing solid-phase tackifying by using a carbon dioxide/steam mixed gas as a protective gas. First, the temperature is raised to (T-70)oAnd C, keeping the temperature for 1-5 hours. Continuously heating to (T-50)oAnd C, keeping the temperature for 1-3 hours. Then cooling to (T-60)oAnd C, keeping the temperature for 1-5 hours. Finally, the temperature is raised to (T-40)oAnd C, keeping the temperature constant until discharging. Wherein T isoCIs the melting point of the resin. And finally, continuously sampling in the constant temperature process, and determining the final polymerization end point by sampling and testing the viscosity.
The polyamide molding composition consisting of the semi-aromatic polyamide comprises the following components in parts by weight:
100 parts of the semi-aromatic polyamide;
10-70 parts of reinforcing filler;
0-40 parts of a toughening agent.
The reinforcing filler is selected from one or more of glass fiber, carbon fiber, asbestos fiber, metal fiber, talc, wollastonite, halloysite, calcite, glass beads, ceramic beads, kaolin, diatomite, mica, calcium carbonate and magnesium salt whisker;
the toughening agent is selected from at least one of a rubber toughening agent and a thermoplastic elastomer toughening agent; the rubber toughening agent comprises one or more of nitrile rubber, ethylene propylene rubber and styrene butadiene rubber; the thermoplastic elastomer toughening agent comprises one or more of styrene toughening agents, polyolefin toughening agents, polyurethane toughening agents and polyester toughening agents.
If a flame retardant effect is required, a certain amount of flame retardant is required to be added. 0-50 parts of flame retardant is also included according to the parts by weight; the halogen flame retardant or the halogen-free flame retardant; preferably, the flame retardant is preferably a halogen-free flame retardant; the halogen flame retardant comprises one or more of chlorinated paraffin, hexachlorocyclopentadiene, tetrachloro-o-dibenzoic anhydride, brominated polystyrene, brominated polyphenyl ether, brominated bisphenol A epoxy resin, brominated styrene-maleic anhydride copolymer, brominated epoxy resin, brominated phenoxy resin, decabromodiphenyl ether, decabromodiphenyl, brominated polycarbonate, pentabromotoluene, hexabromobenzene, 1, 2-bis (dibromonorbornyl dicarboximide) ethane, 2-bis (tetrabromophthalimide) ethane, perbromo-tricyclopentadecane, tetradecbromodiphenoxybenzene and brominated aromatic cross-linked polymer; the halogen-free flame retardant comprises one or more of nitrogen-containing flame retardant, phosphorus-containing flame retardant or nitrogen and phosphorus-containing flame retardant.
The invention has the following beneficial effects
The invention finds that the high-performance polyamide resin with good tinting strength can be obtained by regulating the content of the bio-based carbon, the proportion of the repeating units and the concentration of the end groups.
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The performance test method comprises the following steps:
(1) the content of the bio-based carbon is measured according to ASTM standard D6866-12/Method-B, and the molar content of the bio-based carbon is calculated according to the following formula: the molar content of biobased carbon is (molar biobased carbon/molar total organic carbon) × 100%.
(2) The method for testing the amino content in the obtained semi-aromatic polyamide resin comprises the following steps: the amino content of the sample end was titrated with a Metrohm 848 titroproplus full-automatic potentiometric titrator. 0.5 g of polyamide is taken, 45 mL of phenol and 3mL of anhydrous methanol are added, heating and refluxing are carried out, after a sample is observed to be completely dissolved, the temperature is cooled to room temperature, and the content of terminal amino groups is determined by using a calibrated hydrochloric acid standard solution.
(3) The method for testing the carboxyl content in the obtained semi-aromatic polyamide resin comprises the following steps: the carboxyl content of the sample terminal was titrated with a Metrohm 848 titroproplus full-automatic potentiometric titrator. 0.5 g of polyamide is taken and added with 50 mL of o-cresol for refluxing dissolution, 400 mu L of formaldehyde solution is rapidly added after cooling, and the content of terminal carboxyl is titrated by using a calibrated KOH-ethanol solution.
(4) Method for testing melting point of the obtained semi-aromatic polyamide resin: see ISO11357 (2009). The specific test method comprises the following steps: the melting point and enthalpy of fusion of the sample were measured with a Perkin Elmer Diamond DSC analyzer at a temperature rise rate of 10oC/min。
(5) Characterization method of tinting strength of semi-aromatic polyamide resin and molding composition: and (2) carrying out vacuum drying on the polyamide resin in an oven at the temperature of 100 ℃ for 10 h, respectively mixing 20 parts of modified titanium dioxide and 80 parts of polyamide resin, and carrying out extrusion granulation to obtain the color master batch. The prepared color master batch is used for coloring the polyamide resin or the molding composition thereof and is injected into a color plate product with the pigment content of 0.4 percent. The relative tinting strength values were obtained by comparison using the X-Rite Coloreye 7000A colorimeter according to GB/T11186.2-1989 against comparative example 1.
The examples and comparative examples prepared with polyamide resins used the following raw material sources:
1, 10-decamethylenediamine a: a bio-based;
1, 10-decamethylenediamine B: petroleum-based;
terephthalic acid A: a bio-based;
terephthalic acid B: petroleum-based;
isophthalic acid: petroleum-based;
1, 10-sebacic acid: a bio-based;
adipic acid: a bio-based;
suberic acid: petroleum-based;
1, 12-dodecanedioic acid: a bio-based;
examples and comparative examples preparation of semi-aromatic polyamides:
adding reaction raw materials in a pressure kettle which is provided with a magnetic coupling stirring device, a condenser pipe, a gas phase port, a feeding port and a pressure explosion-proof port according to the proportion shown in the table 1, and then adding sodium hypophosphite, an antioxidant and deionized water, wherein the weight of the sodium hypophosphite is 0.1 percent of the weight of the materials fed except the deionized water, and the weight of the deionized water is 30 percent of the total weight of the materials fed; vacuumizing, filling high-purity argon as a protective gas, and starting to react. And heating the reaction mixture to 190-210 ℃, stirring for 3-5 hours, then opening a valve to slowly release pressure and drain water, and simultaneously keeping the temperature and the pressure unchanged. Directly discharging water until the water discharge amount reaches 70% of the amount of the added deionized water. At the moment, the temperature starts to rise, the temperature rises to 220-240 ℃ within 3 hours, and the temperature is kept constant for 2 hours. And opening a valve to discharge after the reaction is finished to obtain the prepolymer.
Prepolymer in 80oAnd C, after vacuum drying for 24 hours, solid-phase tackifying is carried out by using a mixed gas of carbon dioxide/water vapor as a protective gas. First, the temperature is raised to (T-70)oAnd C, keeping the temperature for 1-5 hours. Continuously heating to (T-50)oAnd C, keeping the temperature for 1-3 hours. Then cooling to (T-60)oAnd C, keeping the temperature for 1-5 hours. Finally, the temperature is raised to (T-40)oAnd C, keeping the temperature constant until discharging. Wherein T isoCIs the melting point of the resin. And finally, continuously sampling in the constant temperature process, and determining the final polymerization end point by sampling and testing the viscosity.
Table 1: examples 1-7 formulations of semi-aromatic polyamides and results of various property tests
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
1, 10-decamethylenediamine A, mol | 20 | 20 | 20 | 20 | 20 | 20 | 20 |
Terephthalic acid A, mol | 14 | 14 | 14 | 14 | 14 | 10.8 | 14 |
Isophthalic acid, mol | 6 | ||||||
1, 10-sebacic acid, mol | 6 | ||||||
Adipic acid, mol | 6 | ||||||
Suberic acid, mol | 6 | ||||||
1, 12-dodecanedioic acid, mol | 6 | 9.2 | 6 | ||||
Relative viscosity | 2.190 | 2.018 | 2.078 | 2.109 | 2.114 | 2.086 | 2.102 |
Melting point of | 274 | 269 | 286 | 275 | 266 | 252 | 264 |
Content of terminal amino groups, mol/ton | 59 | 43 | 41 | 49 | 39 | 46 | 67 |
Content of carboxyl end groups, mol/ton | 78 | 60 | 72 | 80 | 62 | 79 | 134 |
Biobased content,% of | 86.7 | 100 | 100 | 86.7 | 100 | 100 | 100 |
Relative coloring power% | 112 | 113 | 109 | 118 | 120 | 119 | 117 |
From examples 1 to 5, it is clear that the semi-aromatic polyamide containing preferable suberic acid and 1, 12-dodecanedioic acid monomer is more excellent in coloring property.
As is apparent from example 5/6/9/10 and comparative example 5/6, the molar content of the repeating unit needs to fall within the range of the present invention, and the preferable range of the content of the repeating unit is one that can give a polyamide resin having better colorability.
From example 5/7/8, it is clear that the content of the terminal amino group and the terminal carboxyl group has a significant influence on the coloring property of the semi-aromatic polyamide.
Table 2: examples 8-11 formulations of semi-aromatic polyamides and results of various property tests
Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | |
1, 10-decamethylenediamine A, mol | 20 | 20 | 20 | 15 | |
1, 10-decamethylenediamine B, mol | 5 | 20 | |||
Terephthalic acid A, mol | 14 | 12 | 13 | 13.6 | 11 |
Terephthalic acid B, mol | 0.4 | 3 | |||
1, 12-dodecanedioic acid, mol | 6 | 8 | 7 | 6 | 6 |
Relative viscosity | 2.094 | 2.073 | 2.008 | 2.096 | 2.151 |
Melting point of | 271 | 262 | 265 | 272 | 269 |
Content of terminal amino groups, mol/ton | 43 | 60 | 51 | 56 | 42 |
Content of carboxyl end groups, mol/ton | 187 | 79 | 80 | 81 | 89 |
Biobased content,% of | 100 | 100 | 100 | 86.1 | 41.6 |
Relative coloring power% | 116 | 124 | 123 | 113 | 110 |
From example 5/11/12, it is clear that the content of the bio-based carbon has a significant influence on the coloring property of the semi-aromatic polyamide within the range of the present invention, and the coloring property is more preferable when the content of the bio-based carbon exceeds 86%.
Table 2: comparative examples 1 to 4 formulations of semi-aromatic polyamides and results of various property tests
Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
1, 10-decamethylenediamine A, mol | 20 | 20 | 20 | 20 | |||
1, 10-decamethylenediamine B, mol | 20 | 20 | 20 | ||||
Terephthalic acid A, mol | 4 | 14 | 14 | 8 | 16 | 4 | |
Terephthalic acid B, mol | 20 | 10 | 10 | ||||
1, 12-dodecanedioic acid, mol | 6 | 6 | 6 | 12 | 4 | 6 | |
Relative viscosity | 2.110 | 2.010 | 2.021 | 2.056 | 2.091 | 2.074 | 2.081 |
Melting point of | 315 | 270 | 271 | 268 | 245 | 277 | 272 |
Content of terminal amino groups, mol/ton | 58 | 42 | 40 | 180 | 52 | 42 | 167 |
Content of carboxyl end groups, mol/ton | 80 | 71 | 261 | 96 | 67 | 78 | 216 |
Biobased content,% of | 0 | 27.1 | 100 | 100 | 100 | 100 | 27.1 |
Relative coloring power% | 100 | 103 | 104 | 102 | 105 | 103 | 97 |
The relative colorability was determined to be 100% based on the colorability of comparative example 1.
From comparative example 1/2 and example 12, it is understood that even though the molar ratio of each monomer and the content of terminal groups are within the range of the present invention, the biobased content is low and the improvement in the coloring property is limited, the improvement is remarkable when the biobased content is higher than 39 mol%.
From comparative example 3/4, it is understood that the content of terminal groups is outside the range of the present invention and the improvement of colorability is limited.
As can be seen from comparative example 7, when neither the biobased content nor the terminal group content was within the range of the present invention, the coloring property was even worse.
It can be seen from the comprehensive comparison example that in order to achieve the increase of the relative tinting strength, according to the technical scheme of the invention, the molar ratio of each monomer, the content of the terminal amino group and the content of the bio-group are required to reach the range of the invention.
The proportions of the components of the molding compositions of example 5 and comparative example 1/4/6/7, which are composed of polyamide resin, and the preparation method are as follows: 100 parts of polyamide resin; 30 parts of talc; and 15 parts of nitrile rubber.
Method for producing a polyamide molding composition: according to the formula, polyamide resin, talc and butadiene acrylonitrile rubber are uniformly mixed in a high-speed mixer, then the mixture is added into a double-screw extruder through a main feeding port, and a reinforcing filler is fed laterally through a lateral feeding scale, extruded, cooled by water, granulated and dried to obtain the polyamide molding composition.
Table 3: the proportion of the components of the polyamide molding composition
Sources of polyamide resins | Example 5 | Comparative example 1 | Comparative example 4 | Comparative example 6 | Comparative example 7 |
Relative coloring power% | 128 | 104 | 105 | 107 | 99 |
As is apparent from Table 3, the molding compositions obtained according to the present invention are superior in relative tinting strength after the semi-aromatic polyamide resins of the respective examples and comparative examples are prepared into molding compositions.
Claims (10)
1. A semi-aromatic polyamide comprising, based on the molar content of all the recurring units of the chain segment: (a) 53 mol/% -71 mol/% of 10T units derived from 1, 10-decanediamine and terephthalic acid; (b) 29mol/% -47 mol% of 10X units derived from 1, 10-decanediamine and at least one of isophthalic acid, 1, 4-cyclohexanedicarboxylic acid, adipic acid, suberic acid, 1, 10-decanedioic acid, 1, 12-dodecanedioic acid, pentadecanedioic acid; wherein, in the semi-aromatic polyamide, the molar content of the bio-based carbon is 39 mol% -100 mol%; in the semi-aromatic polyamide, the amino content is 30-100 mol/ton, and the carboxyl content is 30-200 mol/ton.
2. Semi-aromatic polyamide according to claim 1, characterized in that the recurring units: (a) 60mol/% -66 mol/% of 10T units; (b) 34 mol/% -40 mol% of 10X units.
3. Semi-aromatic polyamide according to claim 1, characterized in that the 10X units are derived from 1, 10-decamethylenediamine and at least one of 1, 12-dodecanedioic acid, suberic acid.
4. Semi-aromatic polyamide according to claim 1, characterized in that the content of biobased carbon is measured according to ASTM standard D6866-12/Method-B; preferably, the molar content of the bio-based carbon is 86 mol% to 100 mol%.
5. The semi-aromatic polyamide according to claim 1, wherein the semi-aromatic polyamide has an amino group content of 30 to 60 mol/ton and a carboxyl group content of 50 to 80 mol/ton.
6. The semi-aromatic polyamide according to claim 1, characterized in that the biobased carbon is derived from at least one of 1, 10-decanediamine, terephthalic acid, 1, 10-decanedioic acid, 1, 12-dodecanedioic acid, adipic acid.
7. The semi-aromatic polyamide according to claim 1, characterized in that the semi-aromatic polyamide has a melting point of 210 ℃ to 300 ℃.
8. Polyamide moulding compositions consisting of the semi-aromatic polyamides according to any of claims 1 to 7, characterized in that they comprise the following components in parts by weight:
100 parts of the semi-aromatic polyamide according to any one of claims 1 to 7;
10-70 parts of reinforcing filler;
0-40 parts of a toughening agent.
9. Polyamide moulding composition according to claim 8, characterized in that the reinforcing filler is selected from one or more of the group consisting of glass fibres, carbon fibres, asbestos fibres, metal fibres, talc, wollastonite, halloysite, calcite, glass beads, ceramic beads, kaolin, diatomaceous earth, mica, calcium carbonate, magnesium salt whiskers; the toughening agent is selected from at least one of a rubber toughening agent and a thermoplastic elastomer toughening agent; the rubber toughening agent comprises one or more of nitrile rubber, ethylene propylene rubber and styrene butadiene rubber; the thermoplastic elastomer toughening agent comprises one or more of styrene toughening agents, polyolefin toughening agents, polyurethane toughening agents and polyester toughening agents.
10. The polyamide molding composition according to claim 8, further comprising 0 to 50 parts by weight of a flame retardant; the halogen flame retardant or the halogen-free flame retardant; preferably, the flame retardant is preferably a halogen-free flame retardant; the halogen flame retardant comprises one or more of chlorinated paraffin, hexachlorocyclopentadiene, tetrachloro-o-dibenzoic anhydride, brominated polystyrene, brominated polyphenyl ether, brominated bisphenol A epoxy resin, brominated styrene-maleic anhydride copolymer, brominated epoxy resin, brominated phenoxy resin, decabromodiphenyl ether, decabromodiphenyl, brominated polycarbonate, pentabromotoluene, hexabromobenzene, 1, 2-bis (dibromonorbornyl dicarboximide) ethane, 2-bis (tetrabromophthalimide) ethane, perbromo-tricyclopentadecane, tetradecbromodiphenoxybenzene and brominated aromatic cross-linked polymer; the halogen-free flame retardant comprises one or more of nitrogen-containing flame retardant, phosphorus-containing flame retardant or nitrogen and phosphorus-containing flame retardant.
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