CN116285281B - Laser direct structuring thermoplastic compositions containing post consumer recycled polycarbonate and methods of making the same - Google Patents

Laser direct structuring thermoplastic compositions containing post consumer recycled polycarbonate and methods of making the same Download PDF

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Publication number
CN116285281B
CN116285281B CN202211532215.9A CN202211532215A CN116285281B CN 116285281 B CN116285281 B CN 116285281B CN 202211532215 A CN202211532215 A CN 202211532215A CN 116285281 B CN116285281 B CN 116285281B
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polycarbonate
pcr
direct structuring
laser direct
post
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CN116285281A (en
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李莹
吴彤
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Wuxi Yingtong New Material Technology Co ltd
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Wuxi Yingtong New Material Technology Co ltd
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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
    • 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
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/328—Phosphates of heavy metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/20—Recycled plastic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

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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)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a laser direct structuring thermoplastic composition containing Post Consumer Recovery (PCR) polycarbonate, comprising the following components in weight percent: 20 to 60wt% of a polycarbonate; 3-15wt% of a polycarbonate-polysiloxane copolymer; 20-60wt% of a PCR polycarbonate; 1-4wt% of a polyphenolic oxygen resin; 2-10wt% of a laser activatable additive; 5-15wt% of a toughening agent; 0.5-5wt% of other additives. The invention solves the double technical challenges of material toughness and LDS functionality under the condition of using a large amount of post-consumer recovery (PCR) polycarbonate from the aspects of formula design, high performance and functional modification, and prepares the composite material with excellent mechanical property and LDS functionality.

Description

Laser direct structuring thermoplastic compositions containing post consumer recycled polycarbonate and methods of making the same
Technical Field
The invention belongs to the field of functional polymer materials, and particularly relates to a laser direct structuring thermoplastic composition containing post-consumer recovery (PCR) polycarbonate and a preparation method thereof.
Background
In recent years, the polycarbonate productivity in China shows 'blowout rising', the rapid development of the polycarbonate industry is certainly promoted, the self-supporting rate is greatly improved, and the domestic requirement growth is met. Meanwhile, post-consumer recovery (PCR) polycarbonates, including packaging materials, building boards, electrical and electronic housing parts, water tanks, optical media, scrap car lights and other polycarbonate products, have not attracted enough attention in the domestic related industries for their effective recycling. At present, a large amount of PCR materials are recycled and treated by using waste plastics at the low end, the technical content is low, the product quality is unstable, the application requirements at the relatively low end can be met, and the PCR materials are quite far away from the application requirements in the fields of middle-high-end application, particularly high-functional materials.
The principle of the Laser Direct Structuring (LDS) technology is to combine the functions of electric interconnection, supporting components and devices, supporting and protecting the plastic shell, shielding and antenna generated by combining the mechanical entity and the conductive pattern into a whole to form the 3D-MID, which can be used for directly three-dimensionally printing the circuit board on the plastic piece by utilizing the laser technology and is suitable for manufacturing local fine lines. Compared with the traditional circuit board, the LDS technology has the remarkable advantages that the product volume can be effectively reduced, the reliability is improved, and meanwhile, the circuit design is more flexible, so that powerful support is provided for product innovation. The core of LDS engineering plastic preparation is that an auxiliary agent with laser activity is introduced into a matrix, and selective conductive circuit forming is realized by utilizing laser.
The current common laser direct-molding material mainly comprises matrix resin, a laser activatable additive, a toughening agent, an inorganic filler and the like, wherein polycarbonate is common matrix resin. When the recycled polycarbonate material is tried to be directly used for preparing the laser direct structuring material, the stability and toughness of the obtained material are obviously reduced, and the practical requirement cannot be met.
Disclosure of Invention
In view of the above problems, the invention prepares a laser direct structuring thermoplastic composite material containing post-consumer recovery (PCR) polycarbonate from the aspects of formulation design and high performance and functional modification.
On the basis, the obtained high-functionality composite material can be manufactured into various forms of molded products by adopting the technical mode existing in the technical field, thereby meeting the requirements of related applications such as mobile phones, personal computers, communication equipment, medical appliances, automobiles, RFID and the like.
The object of the present invention is to provide a laser direct structuring thermoplastic composition comprising Post Consumer Recycled (PCR) polycarbonate.
In order to achieve the above purpose, the invention adopts the following technical scheme: a laser direct structuring thermoplastic composition comprising post consumer recycled PCR polycarbonate, consisting essentially of the following components in weight percent: 20 to 60wt% of a polycarbonate; 3-15wt% of a polycarbonate-polysiloxane copolymer; 20-60wt% of a PCR polycarbonate; 1-4wt% of a polyphenolic oxygen resin; 2-10wt% of a laser activatable additive; 5-15wt% of a toughening agent; 0.5-5wt% of other additives.
Preferably, the polycarbonate content of the composition is 20-55% by weight.
Preferably, the polycarbonate-polysiloxane copolymer is present in the composition in an amount of 5 to 10 weight percent.
Preferably, the PCR polycarbonate is contained in the composition in an amount of 20 to 50% by weight.
Preferably, the composition contains 1 to 3% by weight of the polyphenylene oxide resin.
Preferably, the composition contains 2-8% by weight of the laser activatable additive; more preferably 3 to 5%.
Preferably, the weight percentage of the toughening agent in the composition is 8-15%; more preferably 9 to 13%.
In the present invention, the polycarbonate comprises a homopolycarbonate having a repeating structure carbonate unit, and may be one or a mixture of two of an aliphatic polycarbonate, a cycloaliphatic polycarbonate or an aromatic polycarbonate. In the present invention, suitable polycarbonates may be prepared by processes such as interfacial polymerization and melt polymerization. In a particular embodiment, the polycarbonate is a linear homopolymer derived from bisphenol A, i.e., a polycarbonate containing bisphenol A structure. The weight average molecular weight of the polycarbonate is from about 18000 to about 35000 as measured by gel permeation chromatography.
Preferably, the polycarbonate is an aromatic polycarbonate containing bisphenol A structure, and the melt index is measured at 300C and 1.2Kg and is 4-25g/10min. As a further preference, the polycarbonate comprises a first polycarbonate having MFR of 15 to 25g/min and a second polycarbonate having MFR of 4 to 10g/min, respectively, at 300℃under 1.2Kg conditions; as a further preferred aspect, the mass ratio of the two polycarbonates is 1:1 to 5.
In the present invention, the polycarbonate-polysiloxane copolymer may comprise 50 to 99 weight percent carbonate units and 1 to 50 weight percent siloxane units. Within this range, the polycarbonate-polysiloxane copolymer may comprise 65 to 99 weight percent carbonate units and 1 to 35 weight percent siloxane units, more specifically 70 to 98 weight percent carbonate units and 2 to 30 weight percent siloxane units, more specifically 2 to 30 weight percent siloxane units, and still more specifically 10 to 30 weight percent siloxane units.
Preferably, the polycarbonate unit in the polycarbonate-polysiloxane copolymer has a polycarbonate unit structure of bisphenol A structure.
Preferably, the weight average molecular weight of the polycarbonate-polysiloxane copolymer is 20000 to 40000.
In the present invention, the post-consumer recycled (PCR) polycarbonate includes packaging materials, building boards, electronic and electrical housing parts, bucket materials, optical media, scrap car lights, and other polycarbonate products, among others. The post-consumer recycled polycarbonates are generally used in the form of recycle particles for actual use. Wherein the reclaimed material particles are obtained through mechanical sorting, cleaning and granulating processes.
In the present invention, the polyphenylene oxide resin contains a repeating unit represented by the following general formula:
Wherein R 1 and R 2 may each represent H, halogen, a C1-C12 alkyl group, or a combination thereof. For example, R 1 and R 2 may each be H, C C3 alkyl groups, particularly methyl, arranged ortho to the hydroxyl group on each arylene group. As a specific preferred embodiment, R 1 and R 2 are H. p and q are each independently integers from 0 to 4. X may be a bridging group linking two hydroxy-substituted aromatic groups (e.g., benzene rings), wherein the bridging group and the hydroxy substituent of each C6 arylene group are arranged ortho, meta, or para to each other on the C6 arylene group. X may be methylene or an alkyl (such as methyl) substituted methylene (-CH (CH 3) 2-). In addition, n is an integer of 1 to 12, and m is an integer of 100 to 300.
In the invention, the polyphenolic oxygen resin is a polyphenolic oxygen resin with a bisphenol A structure. Preferably, the polyphenolic oxygen resin structure is as follows:
preferably, the molecular weight (MW (avg)) of the polyphenylene oxide resin is 30000 to 70000.
Preferably, the polyphenolic oxygen resin is PKHH.
In the present invention, the laser activatable additive is a metal compound and/or metal complex having a spinel or octahedral crystal structure, wherein the content of metal ions in the free state is less than 1ppm and the dielectric loss is <0.005 (frequency 1 MHz). The metal compound may be one or a mixture of at least two of zinc oxide, zinc organic compound, copper oxide, copper organic compound, cobalt oxide, cobalt organic compound, magnesium oxide, magnesium organic compound, tin oxide, tin organic compound, titanium oxide, titanium organic compound, iron oxide, iron organic compound, aluminum oxide, aluminum organic compound, nickel oxide, nickel organic compound, manganese oxide, manganese organic compound, chromium oxide, or chromium organic compound, preferably one or a mixture of at least two of copper oxide, copper organic compound, tin oxide, and tin organic compound; the metal complex is one or a mixture of at least two of zinc complex, copper complex, cobalt complex, magnesium complex, tin complex, titanium complex, iron complex, aluminum complex, nickel complex, manganese complex or chromium complex, preferably one or a mixture of at least two of copper complex and tin complex. Examples of laser direct structuring additives include, but are not limited to, metal oxides, metal oxide coated fillers, and heavy metal mixture oxide spinels, such as copper chromium oxide spinels; copper salts such as basic copper phosphate, copper sulfate, copper thiocyanate; organometallic complexes such as palladium/palladium-containing heavy metal complexes or copper complexes; or combinations comprising at least one of the foregoing LDS additives. Preferably, the laser activatable additive comprises one or more of basic copper phosphate, zinc stannate, tin pyrophosphate, tin phosphate, tin dioxide, stannous pyrophosphate and stannous oxide.
In the invention, the toughening agent is selected from one or more than two of ABS (acrylonitrile-butadiene-styrene copolymer), MBS (methyl methacrylate-butadiene-styrene copolymer), EVA (ethylene-vinyl acetate copolymer), EMA (ethylene-methyl acrylate copolymer), EEA (ethylene-ethyl acrylate copolymer) and EBA (ethylene-butyl acrylate copolymer).
Preferably, the toughening agent is selected from one or more of ABS (acrylonitrile-butadiene-styrene copolymer), MBS (methyl methacrylate-butadiene-styrene copolymer), EMA (ethylene-methyl acrylate copolymer), EBA (ethylene-butyl acrylate copolymer). As a still further preferred aspect, the toughening agent is selected from the group consisting of ABS, MBS, EMA and EBA-GMA (ethylene-butyl acrylate-glycidyl methacrylate copolymer). Preferably, ABS, MBS, EMA and EBA-GMA are added in a mass ratio of 4-8:1-4:1.5:0.5-2; more preferably 5 to 7:2 to 3:1.5:1 to 1.5.
In the present invention, the other additives include a stabilizer (e.g., a heat stabilizer), an antioxidant, a mold release agent, a colorant, an antistatic agent, an anti-drip agent, and combinations of one or more of the foregoing additives. In various embodiments, the antioxidant comprises a primary antioxidant and a secondary antioxidant. In a further embodiment, the antioxidant is present in the system in an amount of about 0.01wt% to about 0.5 wt%. In various embodiments, the stabilizer is present in the system in an amount of 0.01wt% to about 0.5 wt%. In further embodiments, the stabilizer may comprise a heat stabilizer and a light stabilizer. Suitable heat stabilizers include hindered phenols, organic phosphites, phosphates, or combinations comprising at least one of the foregoing heat stabilizers. Suitable mold release agents in the present invention may comprise metal stearates, polyethylene waxes, silicones, and the like, or combinations comprising at least one of the foregoing mold release agents.
A method of making a laser direct structuring thermoplastic composition of a Post Consumer Recovery (PCR) polycarbonate of any of the above embodiments, comprising: according to the metering ratio, the polycarbonate-polysiloxane copolymer, the PCR polycarbonate, the polyphenylene oxide resin, the additive capable of being activated by laser, the toughening agent and other additives are premixed uniformly, and the mixture is extruded, fused, blended, extruded and granulated by an extruder, so that the PCR polycarbonate laser direct structuring composite material with good mechanical property and LDS functionality is obtained.
The beneficial effects of the invention are as follows: from the aspects of formula design, high performance and functional modification, the double technical challenges of material toughness and LDS functionality are solved under the condition of using a large amount of post-consumer recovery (PCR) polycarbonate, and the composite material with excellent mechanical properties and LDS functionality is prepared.
Drawings
FIG. 1 is a chart of ingredients and corresponding performance test data for the examples.
Detailed Description
For a more detailed description of the invention, reference will be made to specific examples.
The polycarbonates used in the comparative examples and examples were commercial bisphenol A Polycarbonate (PC) resin products from Diman, and had MFR of 18g/min (PC-1) and 8g/min (PC-2) at 300℃and 1.2Kg, respectively.
The polycarbonate-polysiloxane copolymers used in the comparative examples and examples were Gansu silver light SL0301 (Si-PC-1) and Korea Sanyang TRIREX ST-3022 PJ (1) (Si-PC-2).
The recovered PC used in the comparative examples and examples was a non-commercial material obtained by crushing and granulating a water tank material (PCR-PC-1) and a recovered optical disk material (PCR-PC-2).
Laser activatable additives used in the comparative and examples include basic copper phosphate (LDS-1), stannous pyrophosphate (LDS-2) and zinc stannate (LDS-3).
The toughening agents used in the comparative examples and examples include: ABS (Korea Jinhu HR 181), MBS (American Dow EXL-2690), AC1330 (American Dow ethylene-methyl acrylate copolymer) and PTW (American Dow ethylene-butyl acrylate-glycidyl methacrylate copolymer).
The polyphenylene oxide resin used in the comparative examples and examples was PKHH from Gabriel corporation of America.
In the comparative example and the example, the total amount of the materials is 10kg, and the rest components in the comparative example and the example comprise an antioxidant (antioxidant 1076 or/and antioxidant 168), a colorant (carbon black) and the like, and the addition amounts are all the prior art.
The components of polycarbonate, polycarbonate-polysiloxane copolymer, PCR polycarbonate, polyphenylene oxide resin, laser activatable additive, toughening agent and other additives are weighed in proportion and put into a high-speed mixer for premixing for 5 minutes at high speed. Adding the premixed raw material mixture in a high-speed mixer through a main feed, and melting, mixing, extruding, cooling, drying and granulating in a double-screw extruder, wherein the screw temperature of the double-screw extruder is controlled between 250 ℃ and 270 ℃. The extruded pellets were then blow dried at 100 ℃ for 4 hours and injection molded to evaluate the properties of the material. The test criteria are as follows:
tensile property test: ASTM D638
Bending performance test: ASTM D790
Impact performance test: ASTM D256
Thermal deformation temperature test: ASTM D648
Plating performance test: ASTM B568 calculates the plating index according to the plating thickness of the test sample and the reference sample, wherein the data set value is between 1 and 10, and 10 corresponds to the situation that the plating performance is optimal. It is generally considered that the index is 9 or more to satisfy the practical requirements.
In fig. 1, comparative example 1 is a polycarbonate to approach 1:1 with the PCR-PC, only MBS is adopted as a toughening agent. It can be seen that the notched impact strength and elongation at break of the composite are both at a lower level. In comparative example 2, with the addition of a certain amount of polycarbonate-polysiloxane copolymer, polyphenylene oxide resin and laser activatable additive, under the condition of adopting ABS and MBS to cooperatively toughen, the toughness of the composite material is improved to a certain extent, but the plating performance of the composite material cannot meet the practical requirements. Surprisingly, the addition of AC1330 and PTW can significantly improve plating performance while improving material toughness (example 1). Further, in examples 2-7, as the addition ratio of the PCR-PC was gradually increased and the combination of the laser activatable additives was changed, the mechanical properties of the composite material and the thermal properties and plating properties were well balanced.

Claims (8)

1. A laser direct structuring thermoplastic composition comprising post consumer recycled PCR polycarbonate, characterized by being made from the following components in weight percent: 20-60 wt% of polycarbonate; 3-15 wt% of a polycarbonate-polysiloxane copolymer; 20-60 wt% of a PCR polycarbonate; 1-4 wt% of a polyphenolic oxygen resin; 2-10 wt% of a laser activatable additive; 5-15 wt% of a toughening agent; 0.5-5 wt% of other additives;
The toughening agent is a mixture of ABS, MBS, EMA, EBA-GMA, and the mass ratio of ABS, MBS, EMA to EBA-GMA is 4-8:1-4:1.5:0.5-2.
2. The laser direct structuring thermoplastic composition comprising post-consumer recycled PCR polycarbonate according to claim 1, wherein the polycarbonate is an aromatic polycarbonate comprising bisphenol a structure, having a melt index of 4-25 g/10min measured at 300 ℃ at 1.2 Kg.
3. The laser direct structuring thermoplastic composition comprising a post-consumer recycled PCR polycarbonate of claim 1, wherein the polycarbonate-polysiloxane copolymer comprises 1 to 50 weight percent siloxane units.
4. The post consumer recycled PCR polycarbonate containing laser direct structuring thermoplastic composition of claim 1, wherein the PCR polycarbonate source comprises one or more of packaging materials, building boards, electronics housing parts, bucket materials, optical media, scrap car lights.
5. The laser direct structuring thermoplastic composition comprising post-consumer recycled PCR polycarbonate of claim 1, wherein the polyphenolic oxygen resin is a polyphenolic oxygen resin having a bisphenol a structure.
6. The post consumer recovery PCR polycarbonate containing laser direct structuring thermoplastic composition of claim 1, wherein the laser activatable additive comprises one or more of basic copper phosphate, zinc stannate, tin pyrophosphate, tin phosphate, tin dioxide, stannous pyrophosphate, stannous oxide.
7. The laser direct structuring thermoplastic composition comprising post-consumer recycled PCR polycarbonate of claim 1, wherein the other additives comprise one or more of stabilizers, mold release agents, colorants, antistatic agents, anti-drip agents.
8. A method for preparing the laser direct structuring thermoplastic composition comprising post-consumer recycled PCR polycarbonate of any of claims 1-7, wherein the polycarbonate, polycarbonate-polysiloxane copolymer, PCR polycarbonate, polyphenylene oxide resin, laser activatable additives, toughening agents and other additives are pre-mixed in a metered ratio, and extruded through an extruder, melt blended, extruded and pelletized to obtain a PCR polycarbonate laser direct structuring composite material with LDS functionality.
CN202211532215.9A 2022-12-01 2022-12-01 Laser direct structuring thermoplastic compositions containing post consumer recycled polycarbonate and methods of making the same Active CN116285281B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033575A (en) * 2017-05-18 2017-08-11 无锡赢同新材料科技有限公司 Laser direct organization polycarbonate Alloys composition, preparation and application
CN114479410A (en) * 2022-02-16 2022-05-13 无锡赢同新材料科技有限公司 LDS (laser direct structuring) engineering plastic with low dielectric loss and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033575A (en) * 2017-05-18 2017-08-11 无锡赢同新材料科技有限公司 Laser direct organization polycarbonate Alloys composition, preparation and application
CN114479410A (en) * 2022-02-16 2022-05-13 无锡赢同新材料科技有限公司 LDS (laser direct structuring) engineering plastic with low dielectric loss and preparation method thereof

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