CN114525018A - Copolyester micro-foaming flame-retardant material and preparation method thereof - Google Patents
Copolyester micro-foaming flame-retardant material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C—CHEMISTRY; METALLURGY
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0028—Use of organic additives containing nitrogen
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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Abstract
The invention relates to a copolyester microcellular foam flame-retardant material and a preparation method thereof, wherein the copolyester microcellular foam flame-retardant material comprises the following components in parts by weight: 100 parts of PCTG; 10-20 parts of a flame retardant (a mixture of brominated epoxy resin, brominated triazine and antimony trioxide); 0.1-0.5 part of foaming agent; the brominated epoxy resin is a compound of EP type brominated epoxy resin and EC type brominated epoxy resin, the weight-average molecular weight of the EP type brominated epoxy resin is 25000-35000, and the weight-average molecular weight of the EC type brominated epoxy resin is more than 9000; the copolyester micro-foaming flame-retardant material has a foam pore diameter of 5-10 μm and a density of 1.0 ℃ -1.1g/cm3(ii) a The preparation method comprises the following steps: the components are mixed by a screw and then melted at a certain temperature, and then carbon dioxide is introduced under pressure for foaming and extrusion molding to obtain the copolyester micro-foaming flame retardant material. The invention realizes the flame-retardant foaming process of the PCTG material, and the final material has good flame retardance, good foaming uniformity, less uniform breakage of foam holes, good workability, low density and better mechanical property.
Description
Technical Field
The invention belongs to the technical field of composite materials, and relates to a copolyester micro-foaming flame-retardant material and a preparation method thereof.
Background
PCTG is an amorphous copolyester, because a certain amount of ethylene glycol in its structure is replaced by Cyclohexanediol (CHDM) (higher than 50%), it can prevent crystallization, further improve processing and transparency, and its product is highly transparent, excellent in impact resistance, especially suitable for forming thick-walled transparent products, its processing and forming properties are excellent, it can be designed into any shape according to the designer's intention, it can adopt traditional forming methods such as extrusion, injection molding, blow molding and plastic suction, it can be widely used in the markets of sheet material, high-performance shrink film, bottle and special-shaped material, cosmetic package, etc., and its secondary processing properties are excellent, it can be processed and modified by conventional machining.
PCTG materials are particularly suitable for applications requiring very low extraction rates, high definition and very high gamma stability. It has high impact properties and many of the characteristics of polycarbonate, and does not contain bisphenol A, BPS or any other bisphenols. The FDA in the united states is about food contact standards, and can be widely applied to the fields of food, medicine, cosmetic packaging, and the like, toys, household utensils, medical supplies, and the like.
The molecular chain activity of the PCTG is reduced due to the high proportion of cyclohexanediol contained in the structure, the influence on foaming is large, particularly after the flame retardant is added, the polyester structure is easily degraded and becomes brittle at high temperature due to the high temperature action of the flame retardant and polyester, and the foamability of the PCTG is poorer, and the conditions of poor uniformity and nonuniform size of cells in the foaming process are further caused due to the change of molecular weight, so that no related technical patent related to PCTG flame-retardant extrusion foaming exists at present. The copolyester PETG material has a structure with a small proportion of cyclohexanediol (the proportion is less than 50%), so that the flame-retardant foaming modification is relatively easy. Such as document 1(PETG continuous extrusion foaming behavior [ J)]Plastic 2012,41(3): 38-41), literature 2 (chain extension tackifying modification of recycled PETG and its foaming performance research [ D]2016, university of Hubei industries) promote foaming of materials by chain extension through tackifying modification. While the proportion of the cyclohexanediol in the molecular structure is higher during the PCTG flame-retardant foamingThe reason is that the movement ability is weakened, the viscosity is greatly reduced after the common flame retardant is added, the control difficulty of the foaming process is high, and the difficulty is higher when the foam holes are easy to break. According to the invention, the flame retardant with epoxy end capping is added to the polymer, so that the flame retardance of the material is realized, the viscosity of the material during foaming can be increased through the epoxy end capping, and the foaming uniformity of the material is improved. Meanwhile, different from the common foaming process, the invention adds a trace amount of foaming agent at the front section of the screw to promote the bubble nucleation process and nucleation uniformity of the material, and avoids passing through supercritical CO at the later stage2The situation of different sizes of the foam holes caused by uneven pressure dispersion after the foaming process is pressurized.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a copolyester micro-foaming flame-retardant material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the copolyester micro-foaming flame-retardant material comprises the following components in parts by weight:
100 parts of PCTG (polyethylene glycol terephthalate-1, 4-cyclohexanedimethanol ester);
10-20 parts of a flame retardant;
0.1-0.5 part of foaming agent;
the flame retardant is a mixture of brominated epoxy resin, brominated triazine (Weifang Weidong chemical industry, RDT-8) and antimony trioxide (PeBai chemical industry antimony trioxide);
the brominated epoxy resin is a compound of EP type brominated epoxy resin and EC type brominated epoxy resin, the weight-average molecular weight of the EP type brominated epoxy resin is 25000-35000 (opening beautifying chemical epoxy resin KBE-2030K), and the weight-average molecular weight of the EC type brominated epoxy resin is more than 9000 (opening beautifying chemical epoxy resin KBE-3010K);
the diameter of the foam hole of the copolyester micro-foaming flame-retardant material is 5-10 mu m, and the density is 1.0-1.1 g/cm3。
As a preferred technical scheme:
according to the copolyester micro-foaming flame-retardant material, the mass ratio of brominated epoxy resin, brominated triazine and antimony trioxide in the flame retardant is 1:2: 1. The bromine content of the brominated triazine is more than 65 percent, the flame retardant efficiency is high, the bromine content of the brominated epoxy resin is 50 percent or lower, so the flame retardant efficiency is slightly poor, but the viscosity of the material is ensured by the high molecular weight of the brominated epoxy resin, meanwhile, the viscosity uniformity and the pore wall support degree of the nucleation growth process of the material are ensured by the cross-linking reaction of an epoxy group and esters, the brominated triazine has high proportion and good flame retardant performance, but the micro-foaming pores are not uniform and are easy to crack, and if the ratio is too low, the flame retardant performance cannot meet the use requirement. Based on the consideration, the brominated epoxy resin, the brominated triazine and the antimony trioxide are compounded, and the compounding mass ratio is 1:2: 1.
According to the copolyester microfoaming flame-retardant material, the mass ratio of the EP type brominated epoxy resin to the EC type brominated epoxy resin is 2:3, so that the flame retardant end-capped epoxy groups are enabled to have a crosslinking effect with polyester at a proper ratio, a proper viscosity is provided, too high viscosity causes too long and slow growth of nucleation time, and too low viscosity causes too fast growth of cells, and the cells are easy to break.
The PCTG is a product obtained by polycondensing three monomers of terephthalic acid (PTA), Ethylene Glycol (EG) and 1, 4-Cyclohexanedimethanol (CHDM) by using an ester exchange method.
The copolyester micro-foaming flame retardant material comprises more than 50% of 1, 4-cyclohexanedimethanol in the ethylene glycol and the 1, 4-cyclohexanedimethanol in molar proportion.
The PCTG has Rockwell hardness (ASTM D785, R-scale) of 105-115 and bending strength of more than 65 MPa.
The copolyester microfoaming flame-retardant material is characterized in that the foaming agent is azodicarbonamide.
The invention also provides a method for preparing the copolyester micro-foaming flame-retardant material, wherein the components are mixed by a screw and then melted at a certain temperature, and then carbon dioxide is introduced under pressure for foaming and extrusion molding to obtain the copolyester micro-foaming flame-retardant material; the pressurizing pressure is 10-15 MPa.
As a preferred technical scheme:
in the process described above, the blowing agent azodicarbonamide is added in the fourth section of the screw and carbon dioxide is introduced under pressure in the eighth section of the screw. The micro azodicarbonamide is uniformly dispersed under the shearing and mixing action of the screw, and uniformly distributed bubble nuclei are generated due to pyrolysis, so that the dissolving difficulty is reduced when carbon dioxide is introduced into the rear section of the screw, the forming and growing speed of bubbles is increased, and the uniformity is ensured.
In the method, the processing temperatures of the sections of the screw are respectively as follows:
the first section is 200 +/-5 ℃;
the second section is 220 +/-5 ℃;
the third section is 220 +/-5 ℃;
the fourth section is 170 +/-5 ℃;
the fifth section is 170 plus or minus 5 ℃;
the sixth section is 140 plus or minus 5 ℃;
the seventh section is 130 +/-5 ℃;
the eighth segment is 130 +/-5 ℃;
the ninth stage is 120 +/-5 ℃. The first half section has higher process temperature, so that the mixing uniformity of the materials is ensured, and the fourth section starts to cool and simultaneously introduces the foaming agent, so that the foaming agent can be mixed and decomposed at the temperature to form micro bubbles. The temperature setting of the second half ensures that the material has a suitable foaming viscosity.
The principle of the invention is as follows:
the EP-type brominated epoxy resin end group contains an epoxy group, the EC-type epoxy resin end-capping agent is tribromophenol, the high molecular weight brominated epoxy resin flame retardant ensures the viscosity of the material, and the brominated epoxy resin flame retardant contains an epoxy group because of partial end capping, so the brominated epoxy resin flame retardant can generate a crosslinking reaction with PCTG at high temperature, thereby ensuring that the integral melt strength of the material is in a proper range and avoiding the cell breakage caused by overlarge bubbles. Meanwhile, different from the common foaming process, the invention adds a trace amount of foaming agent in the front section of the screw to promote the bubble nucleation process and nucleation uniformity of the material, and avoids passing through supercritical CO in the later stage2The situation of different sizes of the foam holes caused by uneven pressure dispersion after the foaming process is pressurized.
Has the advantages that:
(1) the invention realizes the flame-retardant foaming process of the PCTG material, and the final material has good flame retardance, good foaming uniformity, uniform cells, less breakage and good workability;
(2) the micro-foaming flame-retardant polyester material disclosed by the invention is high in notch impact strength and tensile strength, so that the characteristics of the PCTG material are ensured to a certain extent, and the characteristics of low density and light weight are also given. Meanwhile, the material has higher elongation at break, and the impact resistance of the PCTG material is ensured.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The raw materials used in the examples were as follows:
PCTG is Eastman PCTG TX 1001;
the flame retardant is a mixture of brominated epoxy resin, brominated triazine and antimony trioxide, the mass ratio of the brominated epoxy resin to the brominated antimony trioxide is 1:2:1, wherein the brominated triazine is RDT-8 in Weifang-Weidong chemical industry, the antimony trioxide is antimony trioxide in Baiyao chemical industry, the brominated epoxy resin is a compound of EP type brominated epoxy resin and EC type brominated epoxy resin, the EP type brominated epoxy resin is KBE-2030K in Kaimei chemical industry, the EC type brominated epoxy resin is KBE-3010K in Kaimei chemical industry, and the mass ratio of the EP type brominated epoxy resin to the EC type brominated epoxy resin is 2: 3;
the foaming agent is azodicarbonamide and the foaming agent is sold under the trade name of Haili group AC-H802A.
The test standards of the indexes of the examples are as follows:
the density of the copolyester microfoaming flame-retardant material is tested according to the ASTM D792 standard, the diameter of a cell is confirmed by an electron microscope to determine the specific size, the flame-retardant property is tested according to the UL 94 standard, the bending strength is tested according to the ASTM D790 standard, the notch impact strength is tested according to the ASTM D256 standard, and the elongation at break is tested according to the ASTM D638 standard.
Example 1
A preparation method of a copolyester microcellular foam flame-retardant material comprises the following steps:
(1) the processing temperature of each section of the screw is set as follows: a first section of 200 ℃; the second section is 220 ℃; a third section of 220 ℃; a fourth stage of 170 ℃; a fifth stage of 170 ℃; a sixth stage of 140 ℃; a seventh section of 130 ℃; an eighth stage of 130 ℃; a ninth stage of 120 ℃;
(2) feeding and mixing 100 parts by weight of PCTG and 10 parts by weight of flame retardant from a first section of a screw;
(3) after the PCTG and the flame retardant reach the fourth section of the screw rod, 0.1 part by weight of foaming agent is added into the fourth section of the screw rod and mixed with the PCTG and the flame retardant;
(4) after the PCTG, the flame retardant and the foaming agent reach the eighth section of the screw, pressurizing the eighth section of the screw by 10MPa and introducing carbon dioxide to foam the mixed melt;
(5) and extruding and molding the foamed melt to obtain the copolyester micro-foaming flame-retardant material.
The finally prepared copolyester micro-foaming flame-retardant material has the density of 1.1g/cm3, the cell diameter of 5 microns, the flame retardance of V2, the bending strength of 60MPa, the notch impact strength of 350J/m and the elongation at break of 150%.
Example 2
A preparation method of a copolyester micro-foaming flame-retardant material comprises the following steps:
(1) the processing temperature of each section of the screw is set as follows: a first section of 200 ℃; the second section is 220 ℃; a third section of 220 ℃; a fourth stage of 170 ℃; a fifth stage of 170 ℃; a sixth stage of 140 ℃; a seventh section of 130 ℃; an eighth stage of 130 ℃; a ninth stage of 120 ℃;
(2) feeding 100 parts by weight of PCTG and 14 parts by weight of flame retardant from a first section of a screw;
(3) after the PCTG and the flame retardant reach the fourth section of the screw rod, 0.2 part by weight of foaming agent is added into the fourth section of the screw rod and mixed with the PCTG and the flame retardant;
(4) after the PCTG, the flame retardant and the foaming agent reach the eighth section of the screw, pressurizing the eighth section of the screw by 10MPa and introducing carbon dioxide to foam the mixed melt;
(5) and extruding and molding the foamed melt to obtain the copolyester micro-foaming flame-retardant material.
The finally prepared copolyester microcellular foaming flame retardant material has the density of 1.07g/cm3The cell diameter was 8 μm, the flame retardance was V1, the flexural strength was 57MPa, the notched impact strength was 320J/m, and the elongation at break was 110%.
Example 3
A preparation method of a copolyester micro-foaming flame-retardant material comprises the following steps:
(1) the processing temperature of each section of the screw is set as follows: a first section of 195 ℃; a second section of 215 ℃; a third stage of 215 ℃; a fourth stage 165 ℃; a fifth stage 165 ℃; the sixth section is 135 ℃; a seventh section of 125 ℃; an eighth section of 125 ℃; a ninth stage of 115 ℃;
(2) feeding 100 parts by weight of PCTG and 18 parts by weight of flame retardant from a first section of a screw;
(3) after the PCTG and the flame retardant reach the fourth section of the screw rod, 0.3 part by weight of foaming agent is added into the fourth section of the screw rod and mixed with the PCTG and the flame retardant;
(4) after the PCTG, the flame retardant and the foaming agent reach the eighth section of the screw, pressurizing 15MPa at the eighth section of the screw and introducing carbon dioxide to foam the mixed melt;
(5) and extruding and molding the foamed melt to obtain the copolyester micro-foaming flame-retardant material.
The finally prepared copolyester micro-foaming flame-retardant material has the density of 1.08g/cm3The diameter of the cells is 7 mu m, the flame retardance is V0, the bending strength is 45MPa, the notch impact strength is 300J/m, and the elongation at break is 135%.
Example 4
A preparation method of a copolyester micro-foaming flame-retardant material comprises the following steps:
(1) the processing temperature of each section of the screw is set as follows: a first section of 205 ℃; a second section of 225 ℃; a third stage of 225 ℃; a fourth section of 175 ℃; a fifth section of 175 ℃; a sixth section of 145 ℃; the seventh section is 135 ℃; the eighth section is 135 ℃; a ninth stage of 125 ℃;
(2) feeding 100 parts by weight of PCTG and 20 parts by weight of flame retardant from a first section of a screw;
(3) after the PCTG and the flame retardant reach the fourth section of the screw rod, 0.5 part by weight of foaming agent is added into the fourth section of the screw rod and mixed with the PCTG and the flame retardant;
(4) after the PCTG, the flame retardant and the foaming agent reach the eighth section of the screw, pressurizing 15MPa at the eighth section of the screw and introducing carbon dioxide to foam the mixed melt;
(5) and extruding and molding the foamed melt to obtain the copolyester micro-foaming flame-retardant material.
The finally prepared copolyester micro-foaming flame-retardant material has the density of 1.01g/cm3The diameter of the cells is 10 μm, the flame retardance is V0, the bending strength is 55MPa, the notch impact strength is 240J/m, and the elongation at break is 80%.
Claims (10)
1. The copolyester micro-foaming flame-retardant material is characterized by comprising the following components in parts by weight:
100 parts of PCTG;
10-20 parts of a flame retardant;
0.1-0.5 part of foaming agent;
the flame retardant is a mixture of brominated epoxy resin, brominated triazine and antimony trioxide;
the brominated epoxy resin is a compound of EP type brominated epoxy resin and EC type brominated epoxy resin, the weight-average molecular weight of the EP type brominated epoxy resin is 25000-35000, and the weight-average molecular weight of the EC type brominated epoxy resin is more than 9000;
the diameter of the foam hole of the copolyester micro-foaming flame-retardant material is 5-10 mu m, and the density is 1.0-1.1 g/cm3。
2. The copolyester micro-foaming flame-retardant material according to claim 1, wherein the mass ratio of brominated epoxy resin, brominated triazine and antimony trioxide in the flame retardant is 1:2: 1.
3. The copolyester micro-foaming flame retardant material according to claim 1, wherein the mass ratio of the EP type brominated epoxy resin to the EC type brominated epoxy resin is 2: 3.
4. The micro-foamed flame retardant copolyester material according to claim 1, wherein PCTG is a product of polycondensation of three monomers of terephthalic acid, ethylene glycol and 1, 4-cyclohexanedimethanol by a transesterification method.
5. The flame retardant copolyester unfoamed material as claimed in claim 4, wherein the molar fraction of 1, 4-cyclohexanedimethanol in both ethylene glycol and 1, 4-cyclohexanedimethanol is greater than 50%.
6. The micro-foaming flame-retardant copolyester material according to claim 1, wherein the Rockwell hardness of PCTG is 105-115, and the bending strength is more than 65 MPa.
7. The flame retardant copolyester unfoamed material as claimed in claim 1, wherein the foaming agent is azodicarbonamide.
8. The method for preparing the copolyester microfoaming flame-retardant material according to any one of claims 1 to 7, characterized by comprising the following steps: the components are mixed by a screw and then melted at a certain temperature, and then carbon dioxide is introduced under pressure for foaming and extrusion molding to obtain the copolyester micro-foaming flame retardant material; the pressurizing pressure is 10-15 MPa.
9. The process of claim 8 wherein the blowing agent is added in the fourth section of the screw and the carbon dioxide is introduced under pressure in the eighth section of the screw.
10. The method of claim 9, wherein the screw sections are processed at the following temperatures:
the first section is 200 +/-5 ℃;
the second section is 220 +/-5 ℃;
the third section is 220 +/-5 ℃;
the fourth section is 170 +/-5 ℃;
the fifth section is 170 plus or minus 5 ℃;
the sixth section is 140 plus or minus 5 ℃;
the seventh section is 130 +/-5 ℃;
the eighth segment is 130 +/-5 ℃;
the ninth stage is 120 +/-5 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613899A (en) * | 2013-11-15 | 2014-03-05 | 广东聚石化学股份有限公司 | Anti-flaming acrylonitrile-butadiene-styrene (ABS) alloy material and preparation method thereof |
| CN109135085A (en) * | 2018-07-27 | 2019-01-04 | 武汉金发科技有限公司 | A kind of environmental protection flame retardant poly styrene composite material and preparation method thereof |
| CN111154134A (en) * | 2019-12-27 | 2020-05-15 | 华润化学材料科技股份有限公司 | High-toughness amorphous copolyester flame-retardant foam and preparation method thereof |
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2021
- 2021-12-27 CN CN202111609501.6A patent/CN114525018B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613899A (en) * | 2013-11-15 | 2014-03-05 | 广东聚石化学股份有限公司 | Anti-flaming acrylonitrile-butadiene-styrene (ABS) alloy material and preparation method thereof |
| CN109135085A (en) * | 2018-07-27 | 2019-01-04 | 武汉金发科技有限公司 | A kind of environmental protection flame retardant poly styrene composite material and preparation method thereof |
| CN111154134A (en) * | 2019-12-27 | 2020-05-15 | 华润化学材料科技股份有限公司 | High-toughness amorphous copolyester flame-retardant foam and preparation method thereof |
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