CN110845835B - Polycarbonate/polysulfate alloy resin material and preparation method thereof - Google Patents
Polycarbonate/polysulfate alloy resin material and preparation method thereof Download PDFInfo
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- CN110845835B CN110845835B CN201910969355.4A CN201910969355A CN110845835B CN 110845835 B CN110845835 B CN 110845835B CN 201910969355 A CN201910969355 A CN 201910969355A CN 110845835 B CN110845835 B CN 110845835B
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention relates to a polycarbonate/polysulfate alloy resin material and a preparation method thereof, wherein the material comprises the following components in percentage by mass: 1-99% of polycarbonate, 1-99% of polysulfate, 0.1-20% of compatilizer, 0.5-20% of toughening agent, 0.1-5% of lubricant, 0.3-2% of antioxidant and 1-60% of inorganic matter.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of high polymer materials, in particular to a polycarbonate/polysulfate alloy resin material and a preparation method thereof.
[ background of the invention ]
Polycarbonate (PC) is an engineering plastic with excellent comprehensive performance, has good impact resistance, creep resistance, higher tensile strength, excellent dielectric property, good light transmission performance and good color and size stability, and has the defects of poor stress cracking resistance, fatigue resistance, ultraviolet resistance, friction resistance and acid-base corrosion resistance, high melt viscosity of polycarbonate, poor flowability, difficulty in molding and large residual stress after molding.
The Polysulfate (PSE) is a novel polyester engineering plastic, the main structure of which is one or more of bisphenol A, 4' -dihydroxy diphenyl ether, hydroquinone, resorcinol and diphenol, which are connected by sulfate bonds, and the polysulfate plastic has the advantages of excellent comprehensive performance, easy processing, higher mechanical strength, better friction resistance, ultraviolet resistance, excellent strong acid and strong alkali corrosion resistance, but slightly poor toughness.
The PC/PSE alloy is a novel alloy, can combine the excellent characteristics of two materials, and has excellent light transmission, processability, mechanical strength, abrasion resistance and acid-base corrosion resistance, but the material has larger rigidity and insufficient toughness, thereby greatly limiting the application field of the PC/PSE alloy. In addition, since the structure of polysulfate is similar to that of polycarbonate and has good compatibility, but the chemical bond structure is different, further improvement of compatibility is required.
[ summary of the invention ]
In order to solve the problems, the invention provides a polycarbonate/polysulfate alloy resin material which has high strength, acid and alkali corrosion resistance, wear resistance, ultraviolet resistance and easy processing and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a polycarbonate/polysulfate alloy resin material comprises the following components in percentage by mass (w%):
1 to 99 percent of Polycarbonate (PC);
1 to 99 percent of Polysulfate (PSE);
0.1 to 20 percent of compatilizer;
0.5 to 20 percent of toughening agent;
0.1 to 5 percent of lubricant;
0.3 to 2 percent of antioxidant;
1 to 60 percent of inorganic matter.
As a preferred embodiment, further defined is: the material comprises the following components in percentage by mass (w%):
50% -90% of Polycarbonate (PC);
10% -50% of Polysulfate (PSE);
1 to 10 percent of compatilizer;
5 to 10 percent of toughening agent;
0.1 to 1 percent of lubricant;
0.3 to 0.5 percent of antioxidant;
1 to 10 percent of inorganic matter.
As a preferred embodiment, further defined is: the content of the compatilizer, the toughener, the lubricant, the antioxidant and the inorganic matter is based on the total amount of Polycarbonate (PC) and Polysulfate (PSE).
As a preferred embodiment, further defined is: the Polycarbonate (PC) is bisphenol A polycarbonate.
As a preferred embodiment, further defined is: the molecular weight of the bisphenol A polycarbonate is 30000-35000.
As a preferred embodiment, further defined is: the Polysulfate (PSE) is one or a mixture of any more of bisphenol A polysulfate, 4' -dihydroxy diphenyl ether type polysulfate, hydroquinone type polysulfate, biphenol type polysulfate or resorcinol type polysulfate, and the molecular weight is preferably 30000-60000.
As a preferred embodiment, further defined is: the molecular weight of the bisphenol A type polysulfate is 30000-60000.
As a preferred embodiment, further defined is: the compatilizer is styrene-acrylonitrile-glycidyl methacrylate ternary random copolymer (SAG).
As a preferred embodiment, further defined is: the toughening agent is one or a mixture of any more of ethylene-octene copolymer (POE) grafted Glycidyl Methacrylate (GMA) (POE-g-GMA), ethylene-methyl acrylate-glycidyl methacrylate (E-GMA-MA) or methyl methacrylate-butadiene-styrene (MBS).
As a preferred embodiment, further defined is: the lubricant is pentaerythritol stearate (PETS).
As a preferred embodiment, further defined is: the antioxidant is a compound of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate antioxidant 1076 and tris [2, 4-di-tert-butylphenyl ] phosphite antioxidant 168, and the ratio of the two is 1: 6.
As a preferred embodiment, further defined is: the inorganic matter is calcium carbonate particles with the diameter less than 2.5 mu m.
A method for preparing a polycarbonate/polysulfate alloy resin material, the method comprising the steps of:
step 1: drying Polycarbonate (PC) in a 120 ℃ oven for 4h, drying Polysulfate (PSE) in a 90 ℃ oven for 4h, and weighing the following components in percentage by mass (w%) to obtain the required raw materials;
1 to 99 percent of Polycarbonate (PC);
1 to 99 percent of Polysulfate (PSE);
0.1 to 20 percent of compatilizer;
0.5 to 20 percent of toughening agent;
0.1 to 5 percent of lubricant;
0.3 to 2 percent of antioxidant;
1 to 60 percent of inorganic matter;
step 2: putting the raw materials of the components weighed in the step 1 into a high-speed mixer, and mixing for 5 minutes under the conditions of 400-500rpm to obtain a mixed material;
and step 3: and putting the mixed material into a double-screw extruder, melting, blending and extruding at 190-250 ℃, cooling and granulating to obtain PC/PSE alloy resin particles.
As a preferred embodiment, further defined is: weighing the required raw materials of each component according to the following mass percentage (w%) in the step 1;
50% -90% of Polycarbonate (PC);
10% -50% of Polysulfate (PSE);
1 to 10 percent of compatilizer;
5 to 10 percent of toughening agent;
0.1 to 1 percent of lubricant;
0.3 to 0.5 percent of antioxidant;
1 to 10 percent of inorganic matter.
The beneficial effects of the invention are as follows: 1. polycarbonate (PC) has excellent light transmission and mechanical properties, and by adding Polysulfate (PSE) and combining the excellent properties of two materials, the acid and alkali resistance and the friction resistance of Polycarbonate (PC) can be effectively improved, the mechanical strength is improved, the light transmission is not influenced, the application range is widened, and the PC/PSE alloy resin material is easier to mold and process.
2. The epoxy group in the compatilizer can react with the terminal hydroxyl and carboxyl of the Polycarbonate (PC) and the terminal hydroxyl of the Polysulfate (PSE), so that the binding force of the Polycarbonate (PC) and the Polysulfate (PSE) is improved, and the impact resistance of the blend is obviously improved on the premise of not influencing the processing performance.
3. The elastomer toughening agent is one or a mixture of any more of ethylene-octene copolymer (POE) grafted Glycidyl Methacrylate (GMA) (POE-g-GMA) and ethylene-methyl acrylate-glycidyl methacrylate (E-GMA-MA) with epoxy groups, or a core-shell structure elastomer toughening agent is selected for synergistic toughening, so that the toughening effect and the stability of material performance are ensured.
[ detailed description ] embodiments
The present invention is further illustrated in detail below with reference to examples 1 to 6, comparative example 1 and comparative example 2:
in examples 1 to 6, Polycarbonate (PC) was dried in a 120 ℃ oven for 4 hours, Polysulfate (PSE) was dried in a 90 ℃ oven for 4 hours, the required raw materials of each component were weighed according to the mass percentages in Table 1, and the weighed raw materials of each component were put into a high-speed mixer and mixed for 5 minutes at 400-; and putting the mixed material into a double-screw extruder, melting, blending and extruding at 190-250 ℃, cooling and granulating to obtain PC/PSE alloy resin particles.
Comparative example 1 Polycarbonate (PC) was dried in a 120 ℃ oven for 4 hours, placed in a twin screw extruder, melted and extruded at 190 ℃ to 250 ℃, cooled and pelletized to produce polycarbonate resin pellets.
Comparative example 2, Polysulfate (PSE) is dried in a 90 ℃ oven for 4 hours and then put into a double-screw extruder, melted and extruded at 180-220 ℃, and then cooled and granulated to prepare the polysulfate resin particles.
The obtained PC/PSE alloy resin particles of examples 1 to 6, the polycarbonate resin particles of comparative example 1, and the polysulfate resin particles of comparative example 2 were subjected to a tensile strength property test, a bending strength property test, a notched impact strength property test, a liquid chemical resistance property test, and a hardness property test, respectively.
Tensile strength was tested according to GB/T1040.2-2006.
The flexural strength was tested according to GB/T9341-2008.
Notched impact strength was tested in accordance with GB/T1843-2008.
Liquid chemical resistance was tested according to GB/T11547-2008.
Hardness test the hardness test was carried out according to GB/T230.2-2002.
The test results are shown in tables 1 to 5 below.
Table 1 shows the results of the mechanical property tests of examples 1-6, comparative example 1 and comparative example 2, as follows:
as can be seen from table 1, the preparation of PC/PSE alloy resin material can significantly improve the tensile strength, elastic modulus and hardness of Polycarbonate (PC), and examples 1 and 2 do not add a compatibilizer, so that the toughness of the alloy is slightly reduced because the Polythioester (PSE) material has high rigidity and has a certain compatibility with Polycarbonate (PC), but has a difference in molecular chain structure.
After the compatilizer is added, the comprehensive performance of the alloy is improved, and particularly the notch impact strength and the elongation at break are obviously improved, because the thickness of an interface layer is increased after the compatilizer is added, the coagulation of various dispersed phases is prevented, the compatibility of Polycarbonate (PC) and Polysulfate (PSE) is increased, the bonding force between two phases is increased, a stable phase structure is formed, and the impact resistance of the PC/PSE alloy can be obviously improved.
Analysis of examples 1, 4 and 5 shows that after adding the elastomer toughener POE-g-GMA or the inorganic rigid particles into the blend, the flexibility and the impact resistance of the blend can be significantly improved, because Glycidyl Methacrylate (GMA) has higher reactivity, and the epoxy functional group reacts with the terminal hydroxyl group of the alloy resin after ring opening and is grafted to the main chain, so that the purposes of reactive compatibilization and toughening are achieved, the sensitivity of the alloy resin to the notch strength is effectively improved, and the impact resistance is also improved without affecting the tensile and bending properties of the alloy by adding the elastomer and the inorganic rigid particles.
Analysis of examples 1, 2, 5 and 6 shows that the properties of the alloy resin change significantly when the contents of Polycarbonate (PC) and Polysulfate (PSE) are changed, the material toughness is better and the impact resistance is better when the content of Polycarbonate (PC) is higher, and the material tensile strength, elastic modulus, flexural strength, flexural modulus and hardness are increased and the toughness is decreased when the content of Polysulfate (PSE) is higher.
The PC/PSE alloy resin material can adjust the proportion of each component according to different application field ranges.
Table 2 shows the results of the mechanical properties of the polycarbonate resin pellets obtained in comparative example 1 after being immersed in strong acid and strong base for 7 days, which are as follows:
as can be seen from Table 2, the mechanical properties of Polycarbonate (PC) are greatly reduced in strong acid and strong base, especially in concentrated sulfuric acid, which indicates that Polycarbonate (PC) is not resistant to corrosion by strong acid and strong base.
Table 3 shows the results of the mechanical property test of the polythioester resin particles obtained in comparative example 2 after being soaked in strong acid and strong base for 7 days, which are as follows:
as can be seen from table 3, the mechanical properties of the Polysulfate (PSE) were not changed in various strong acids and bases, indicating that the Polysulfate (PSE) has excellent resistance to strong acids and bases.
Table 4 shows the mechanical property test results of the PC/PSE alloy resin particles obtained in example 1 after being soaked in strong acid and strong base for 7 days, which are as follows:
as can be seen from Table 4, after 10% of Polysulfate (PSE) is added and blended, the PC/PSE alloy resin particles have better retention rate of various mechanical properties after being soaked in strong acid and strong base, and the strong acid and alkali resistance is obviously improved.
Table 5 shows the mechanical property test results of the PC/PSE alloy resin particles obtained in example 2 after being soaked in strong acid and strong base for 7 days, which are as follows:
as can be seen from Table 5, after 20% of Polysulfate (PSE) is added and blended, the PC/PSE alloy resin particles have greatly improved tolerance to strong acid and strong base, have better mechanical property retention rate, and can solve the problem that Polycarbonate (PC) is not acid-base resistant.
Claims (14)
1. The polycarbonate/polysulfate alloy resin material is characterized by comprising the following components in percentage by mass:
1 to 99 percent of polycarbonate;
1 to 99 percent of polysulfate;
0.1 to 20 percent of compatilizer;
0.5 to 20 percent of toughening agent;
0.1 to 5 percent of lubricant;
0.3 to 2 percent of antioxidant;
1 to 60 percent of inorganic matter;
the sum of all components in the material does not exceed 100%.
2. The polycarbonate/polysulfate alloy resin material according to claim 1, characterised in that it comprises the following composition in mass%:
50% -90% of polycarbonate;
10 to 50 percent of polysulfate;
1 to 10 percent of compatilizer;
5 to 10 percent of toughening agent;
0.1 to 1 percent of lubricant;
0.3 to 0.5 percent of antioxidant;
1 to 10 percent of inorganic matter;
the sum of all components in the material does not exceed 100%.
3. The polycarbonate/polysulfate alloy resin material of claim 2, wherein said polycarbonate is selected from the group consisting of bisphenol a polycarbonate.
4. The polycarbonate/polysulfate alloy resin material as set forth in claim 3, wherein the molecular weight of the bisphenol A polycarbonate is 30000-35000.
5. The polycarbonate/polysulfate alloy resin material of claim 2, wherein the polysulfate is selected from one or a mixture of any of bisphenol A polysulfate, 4' -dihydroxydiphenyl ether polysulfate, hydroquinone polysulfate, biphenol polysulfate or resorcinol polysulfate.
6. The polycarbonate/polysulfate alloy resin material according to claim 5, wherein the molecular weight of the bisphenol A polysulfate is 30000 to 60000.
7. The polycarbonate/polysulfate alloy resin material of claim 2, wherein said compatibilizer is a styrene-acrylonitrile-glycidyl methacrylate terpolymer.
8. The polycarbonate/polysulfate alloy resin material of claim 2, wherein the toughening agent is selected from one or a mixture of any of ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-methyl acrylate-glycidyl methacrylate or methyl methacrylate-butadiene-styrene.
9. The polycarbonate/polysulfate alloy resin material as defined in claim 2, wherein said lubricant is selected from pentaerythritol stearate.
10. The polycarbonate/polysulfate alloy resin material of claim 2, wherein the antioxidant is selected from the group consisting of a combination of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) octadecyl propionate antioxidant 1076 and tris [2, 4-di-tert-butylphenyl ] phosphite antioxidant 168.
11. The polycarbonate/polysulfate alloy resin material of claim 10, wherein the beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester antioxidant 1076 and tris [2, 4-di-tert-butylphenyl ] phosphite antioxidant 168 are compounded in a ratio of 1: 6.
12. The polycarbonate/polysulfate alloy resin material as defined in claim 2, wherein said inorganic substance is selected from calcium carbonate particles having a diameter of less than 2.5 μm.
13. A method for preparing the polycarbonate/polysulfate alloy resin material defined in any one of claims 1 to 12, comprising the steps of:
step 1: drying polycarbonate in a 120 ℃ drying oven for 4h, drying polysulfate in a 90 ℃ drying oven for 4h, and weighing the following components in percentage by mass to obtain required raw materials;
1 to 99 percent of polycarbonate;
1 to 99 percent of polysulfate;
0.1 to 20 percent of compatilizer;
0.5 to 20 percent of toughening agent;
0.1 to 5 percent of lubricant;
0.3 to 2 percent of antioxidant;
1 to 60 percent of inorganic matter;
the sum of all components in the material does not exceed 100%;
step 2: putting the raw materials of the components weighed in the step 1 into a high-speed mixer, and mixing for 5 minutes under the conditions of 400-500rpm to obtain a mixed material;
and step 3: and putting the mixed materials into a double-screw extruder, melting, blending and extruding the materials at 190-250 ℃, cooling the materials, and then granulating the materials to obtain the polycarbonate/polysulfate alloy resin particles.
14. The method for preparing a polycarbonate/polysulfate alloy resin material according to claim 13, wherein the required raw materials of the components are obtained in step 1 by weighing:
50% -90% of polycarbonate;
10 to 50 percent of polysulfate;
1 to 10 percent of compatilizer;
5 to 10 percent of toughening agent;
0.1 to 1 percent of lubricant;
0.3 to 0.5 percent of antioxidant;
1 to 10 percent of inorganic matter;
the sum of all components in the material does not exceed 100%.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886808A (en) * | 2003-09-29 | 2006-12-27 | 通用电气公司 | Conductive thermoplastic compositions, methods of manufacture and articles derived from such compositions |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886808A (en) * | 2003-09-29 | 2006-12-27 | 通用电气公司 | Conductive thermoplastic compositions, methods of manufacture and articles derived from such compositions |
Non-Patent Citations (3)
| Title |
|---|
| "Bifloride-catalysed sulfur(VI) fluoride exchange reaction for the synthesis of polysulfates and polysulfonates";Bing Gao et al;《nature chemistry》;20170619;第1-6页 * |
| "SuFEx-Based Synthesis of Polysulfates";Jiajia Dong et al;《Angew Chem Int Ed Engl》;20140901;第53卷(第36期);第9466–9470页 * |
| "新型功能聚硫酸酯材料的高效制备方法及其在电存储器件中应用研究";吴斌;《中国优秀硕士学位论文全文数据库 信息科技辑》;20180615(第06期);I137-53 * |
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