WO2020134843A1 - 一种聚碳酸酯组合物及其制备方法和应用 - Google Patents
一种聚碳酸酯组合物及其制备方法和应用 Download PDFInfo
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- WO2020134843A1 WO2020134843A1 PCT/CN2019/121727 CN2019121727W WO2020134843A1 WO 2020134843 A1 WO2020134843 A1 WO 2020134843A1 CN 2019121727 W CN2019121727 W CN 2019121727W WO 2020134843 A1 WO2020134843 A1 WO 2020134843A1
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- WIPO (PCT)
- Prior art keywords
- polycarbonate
- weight
- stearate
- lubricants
- parts
- Prior art date
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Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/30—Applications used for thermoforming
-
- 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
-
- 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
Definitions
- the invention relates to the technical field of polymer composite materials, in particular to a polycarbonate composition and a preparation method and application thereof.
- PC polycarbonate
- High-viscosity polycarbonate has good toughness, but poor processability due to low fluidity. It is a well-known practice to add low-molecular-weight polyesters to improve overall fluidity. However, this method of improving fluidity will cause other components in the composition, such as fillers and flame retardants, to be difficult to uniformly disperse in the overall composition system due to self-polymerization. The uneven flow leads to poor melt uniformity and toughness of the product, corresponding to poor flame retardant effect and poor overall performance.
- the purpose of the present invention is to overcome the above technical defects and provide a polycarbonate composition, which has the advantages of high transparency, good extrusion melt uniformity and the like.
- Another object of the present invention is to provide a method for preparing the above polycarbonate composition and its application.
- a polycarbonate composition in parts by weight, including 100 parts of polycarbonate; wherein, based on the total weight percentage of polycarbonate, the polycarbonate consists of 10-40% weight average molecular weight of 18000-25000 One polycarbonate, 20-60% second polycarbonate with a weight average molecular weight of 27000-35000, and 20-60% third polycarbonate with a branching degree of 2-7 and a weight average molecular weight of 25000-30000.
- Polycarbonate can be interfacially reacted with a basic aqueous solution of a certain amount of dihydric phenol or a combination of dihydric phenol or an inert solvent of phosgene in the presence of one or more catalysts, or through a Or a variety of aromatic dihydroxy compounds and carbonic acid diester transesterification reaction to produce.
- the one or more dihydroxy aromatic compounds that can be used in the transesterification reaction can include a dihydric phenol, or a combination of dihydric phenols, or a bisphenol, or a combination of bisphenols, or one or more dihydric phenols and A combination of one or more bisphenols.
- dihydric phenols include, but are not limited to resorcinol, resatecinol, catechol, hydroquinone, or 2- Methylhydroquinone (2-methylhydroquioninone) and similar substances.
- bisphenols include, but are not limited to bisphenol A (BPA), 4,4'-dihydroxybiphenyl, 1,1-bis(4-dihydroxy-3-methylphenyl)cyclohexane, 4,4 '-(1-phenylethylidene)bisphenol, 4,4'-dihydroxydiphenylsulfone, 4,4'-cyclohexylidenebisphenol and similar substances.
- commonly used carbonic acid diester reactants include diaryl carbonates, such as diphenyl carbonate (DPC), or activated diaryl carbonates, such as dimethyl salicyl carbonate (BMSC).
- the weight average molecular weight of polycarbonate can be controlled by adding molecular chain regulators with certain functional groups, such as phenolic compounds or alkylphenols, especially phenol, tertiary phenol, cumylphenol, isooctyl One or a combination of phenol and the like is added at a specific time during the polymerization reaction to control the weight average molecular weight of the final product.
- molecular chain regulators with certain functional groups such as phenolic compounds or alkylphenols, especially phenol, tertiary phenol, cumylphenol, isooctyl
- the degree of branching refers to the number of heavy branching points per unit volume or the average relative molecular weight of the branching points.
- Branched polycarbonate is a polyfunctional organic compound added during polymerization: a mixture of hydroxyl, carboxyl, carboxylic anhydride, haloformyl, and the above functional groups.
- it may include trimellitic acid, trimellitic anhydride, trimellitic chloride (trimellitic trichloride), tri-p-hydroxybenzene ethane, isatin bisphenol, triphenol TC (1,3,5-tris ((p-hydroxyphenyl) Isopropyl)benzene), triphenol PC (4(4(1,1-bis(p-hydroxyphenyl)-ethyl) ⁇ , ⁇ -dimethylbenzyl)phenol), 4-chloroformyl ortho Phthalic anhydride, trimesic acid, benzophenone tetracarboxylic acid, 1,1,1-tris(hydroxyphenyl)ethane (THPE), triethylamine, etc.
- the above-mentioned multifunctional organic compound is also called a branch
- the branched polycarbonate can be prepared by introducing a branching agent as a dissolved component in the solvent into the melting process.
- branching agents that generally exhibit a relatively high melting point can be introduced as reactants into the melt polymerization process without the need for the increased amount of energy normally required to melt the branching agent monomer, so that It is in a molten state during the melting process before reacting with other polycarbonate forming reactants.
- the branching agent, diphenol and molecular weight regulator may be added to the alkaline aqueous phase in advance at a predetermined ratio, or dissolved in the organic phase.
- the amount of the branching agent added may be calculated according to the amount of branching desired in the final branched polycarbonate, or a terminating agent or a blocking agent may be added during the reaction to terminate the reaction.
- the first polycarbonate and the second polycarbonate may be linear or branched; preferably, the first polycarbonate and the second polycarbonate are linear.
- the polycarbonate is selected from polycarbonate synthesized by an interfacial method. Since the polycarbonate synthesized by the interfacial method uses phosgene, the characteristic peak of chloride ion can be detected according to the polycarbonate volatile matter test method described below.
- Polycarbonate volatile content test method including the following steps:
- the temperature of desorption and enrichment is 100-140°C, and the time of desorption and enrichment is 1-3 hours. If the desorption temperature is too high, some structurally unstable components will undergo irreversible changes that affect the judgment of the final result; if the desorption temperature is too low, it will not be enough to allow the volatiles to volatilize, such as phenol.
- the enrichment temperature is 30-50°C lower than the desorption temperature.
- the enrichment temperature is 30-50 degrees lower than the desorption temperature in order to completely retain all components.
- the preferred chromatography column of the gas-mass spectrometer is a siloxane column
- the column temperature can be up to 300°C
- the elution temperature is 25°C-300°C
- the elution time is 30-90min.
- Polysiloxane columns containing a certain amount of phenyl content are not likely to tail the volatile substances of polycarbonate, and the separation effect of siloxanes is good.
- the lubricants are selected from stearate lubricants, fatty acid lubricants, and stearate lubricants.
- the stearate lubricant is selected from at least one of calcium stearate, magnesium stearate, and zinc stearate
- the fatty acid lubricant is selected from fatty acids, fatty acid derivatives, At least one fatty acid ester
- the stearate lubricant is selected from at least one of glyceryl monostearate and pentaerythritol stearate;
- it is at least one selected from stearate lubricants.
- the light transmittance of the polycarbonate composition indicates the refractive index of the microstructure inside the material and the number and degree of dispersion of the low-light-transmitting structure. If the refractive index of the internal microstructure of the material is uniform, the low-light-transmitting structure is less and the distribution is uniform , The overall light transmittance of the material is high.
- a method for preparing the above-mentioned polycarbonate composition includes the following steps: mixing polycarbonate and lubricant in a high-mixer according to the ratio, and then adding it to a twin-screw extruder at 240°C- Melt mixing was performed at a temperature of 260°C, and then pelletized, cooled, and dried to obtain a polycarbonate composition.
- the present invention solves the defect of poor melt uniformity of the product after mixing low-viscosity and high-viscosity polycarbonate by adding a third polycarbonate with a branching degree of 2-7 and a weight average molecular weight of 25000-30000, and, because With a certain degree of branching, the free volume inside the material is filled uniformly, reducing or even eliminating the phenomenon of uneven refractive index of the internal structure of the material, so transparency is increased (transparency is a comprehensive indicator of light transmittance and haze, transparency The higher, the smaller the haze, the higher the light transmittance).
- the sources of raw materials used in the present invention are as follows, but are not limited by the following raw materials.
- the first polycarbonate A weight-average molecular weight of 20,000, linear, synthesized by interface method
- the first polycarbonate B weight average molecular weight is 20,000, branching degree is 5, synthesis by interface method;
- Second polycarbonate weight average molecular weight is 33000, linear, synthesized by interface method
- Third polycarbonate weight average molecular weight is 27000, branching degree is 5, synthesis by interface method;
- Polycarbonate C weight average molecular weight 27,000, no branching, synthesis by interface method
- Lubricant A Glycerol monostearate; Fine Organic, stearate lubricant;
- Lubricant B zinc phosphate stearate; Fine Organic, stearate lubricant;
- Antioxidant ADEKA 2112, Edico;
- the preparation method of the polycarbonate composites of the examples and comparative examples the polycarbonate, lubricant and antioxidant are mixed evenly in the high mixer according to the ratio, and then added to the twin screw extruder at 240 °C- It is melt-mixed at a temperature of 260°C, and then pelletized, cooled, and dried to obtain a polycarbonate composite material.
- Extrusion melting uniformity 600 mesh screen is added at the extrusion screw die, and the uniformity is evaluated by the fluctuation of extrusion pressure. The smaller the value, the better the extrusion melting uniformity.
- Example 4/6 It can be seen from Example 4/6 that when the first polycarbonate is linear, transparency and extrusion melt uniformity are better.
- Example 7/8 and Example 4 It can be seen from Example 7/8 and Example 4 that the addition of lubricant will not only improve the extrusion melt uniformity, but also improve the transparency to a certain extent; and the preferred lubricants have a better transparency effect and extrusion melt uniformity Improve better.
- Example 4 It can be seen from Example 4 and Comparative Examples 1-6 that regardless of whether the three polycarbonates are compounded in pairs or added separately, the performance is very poor, and the compounding of the three polycarbonates is required to achieve good performance .
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
Claims (8)
- 一种聚碳酸酯组合物,其特征在于,按重量份计,包括聚碳酸酯100份;其中,基于聚碳酸酯的总重量百分比计,聚碳酸酯由10-40%的重均分子量为18000-25000的第一聚碳酸酯、20-60%的重均分子量为27000-35000的第二聚碳酸酯、20-60%的支化度为2-7重均分子量为25000-30000的第三聚碳酸酯。
- 根据权利要求1所述的聚碳酸酯组合物,其特征在于,所述的第一聚碳酸酯、第二聚碳酸酯为直链的。
- 根据权利要求2所述的聚碳酸酯组合物,其特征在于,所述的聚碳酸酯选自界面法合成的聚碳酸酯。
- 根据权利要求1所述的聚碳酸酯组合物,其特征在于,按重量份计,还包括0.01-4份的润滑剂;所述的润滑剂选自硬脂酸盐类润滑剂、脂肪酸类润滑剂、硬脂酸酯类润滑剂中的至少一种;所述的硬脂酸盐类润滑剂选自硬脂酸钙、硬脂酸镁、硬脂酸锌中的至少一种;所述的脂肪酸类润滑剂选自脂肪酸、脂肪酸衍生物、脂肪酸酯中的至少一种;所述的硬脂酸酯类润滑剂选自单硬脂酸甘油酯、季戊四醇硬脂酸酯中的至少一种。
- 根据权利要求4所述的聚碳酸酯组合物,其特征在于,所述的润滑剂选自硬脂酸酯润滑剂中的至少一种。
- 根据权利要求1所述的聚碳酸酯组合物,其特征在于,按重量份计,还包括0-5份的抗氧剂、耐候剂中的至少一种。
- 一种制备权利要求4所述的聚碳酸酯组合物的制备方法,其特征在于,包括以下步骤:按照配比将聚碳酸酯、润滑剂在高混机中混合均匀,再加入到双螺杆挤出机中,在240℃-260℃的温度下进行熔融混合,然后造粒、冷却、干燥得到聚碳酸酯组合物。
- 权利要求1-6任一项所述的聚碳酸酯复合材料的应用,其特征在于,用于制备透明制件。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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JP2021537191A JP2022515279A (ja) | 2018-12-25 | 2019-11-28 | ポリカーボネート組成物、その製造方法及び使用 |
US17/417,773 US20220073736A1 (en) | 2018-12-25 | 2019-11-28 | Polycarbonate composition, preparation method and application thereof |
EP19905596.3A EP3889219A4 (en) | 2018-12-25 | 2019-11-28 | POLYCARBONATE COMPOSITION, METHOD FOR PREPARATION AND USE THEREOF |
KR1020217022192A KR102631636B1 (ko) | 2018-12-25 | 2019-11-28 | 폴리카보네이트 조성물 및 그 제조 방법과 응용 |
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CN201811589524.3A CN109796736B (zh) | 2018-12-25 | 2018-12-25 | 一种聚碳酸酯组合物及其制备方法和应用 |
CN201811589524.3 | 2018-12-25 |
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WO2020134843A1 true WO2020134843A1 (zh) | 2020-07-02 |
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PCT/CN2019/121727 WO2020134843A1 (zh) | 2018-12-25 | 2019-11-28 | 一种聚碳酸酯组合物及其制备方法和应用 |
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US (1) | US20220073736A1 (zh) |
EP (1) | EP3889219A4 (zh) |
JP (1) | JP2022515279A (zh) |
KR (1) | KR102631636B1 (zh) |
CN (1) | CN109796736B (zh) |
WO (1) | WO2020134843A1 (zh) |
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CN109796736B (zh) * | 2018-12-25 | 2021-05-18 | 金发科技股份有限公司 | 一种聚碳酸酯组合物及其制备方法和应用 |
CN111087785B (zh) * | 2019-12-16 | 2022-05-31 | 金发科技股份有限公司 | 一种透明阻燃聚碳酸酯复合材料及其制备方法 |
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2018
- 2018-12-25 CN CN201811589524.3A patent/CN109796736B/zh active Active
-
2019
- 2019-11-28 WO PCT/CN2019/121727 patent/WO2020134843A1/zh unknown
- 2019-11-28 JP JP2021537191A patent/JP2022515279A/ja active Pending
- 2019-11-28 US US17/417,773 patent/US20220073736A1/en not_active Abandoned
- 2019-11-28 EP EP19905596.3A patent/EP3889219A4/en active Pending
- 2019-11-28 KR KR1020217022192A patent/KR102631636B1/ko active IP Right Grant
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Also Published As
Publication number | Publication date |
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KR20210104804A (ko) | 2021-08-25 |
JP2022515279A (ja) | 2022-02-17 |
CN109796736B (zh) | 2021-05-18 |
EP3889219A4 (en) | 2022-01-12 |
CN109796736A (zh) | 2019-05-24 |
US20220073736A1 (en) | 2022-03-10 |
KR102631636B1 (ko) | 2024-01-30 |
EP3889219A1 (en) | 2021-10-06 |
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