CN116589738A - High-filling waste printed circuit board nonmetal powder polymer composite material with phase change characteristic and preparation method thereof - Google Patents
High-filling waste printed circuit board nonmetal powder polymer composite material with phase change characteristic and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
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- 238000005187 foaming Methods 0.000 claims description 2
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- XBKSAWQCFGREFJ-UHFFFAOYSA-N 3-chloro-n-(4,6-dimethylpyridin-2-yl)benzamide Chemical compound CC1=CC(C)=NC(NC(=O)C=2C=C(Cl)C=CC=2)=C1 XBKSAWQCFGREFJ-UHFFFAOYSA-N 0.000 description 1
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- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C08J9/04—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
- 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
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2427/06—Homopolymers or copolymers of vinyl chloride
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- 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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Abstract
The invention discloses a high-filling waste printed circuit board nonmetal powder polymer composite material with phase change characteristics and a preparation method thereof. The method comprises the steps of mixing NPCB, a high molecular polymer, a processing aid thereof and a phase change material, carrying out open mill, placing the blend in a mould, carrying out hot press molding, and curing to obtain the composite material. The composite material prepared by the method realizes the high doping of NPCB, provides a method for recycling NPCB in a large scale, has good bending property and thermal stability, and also has phase change characteristics in part.
Description
Technical Field
The invention belongs to the technical field of recovery of nonmetal powder of waste printed circuit boards, and particularly relates to a high-filling polymer composite material of Nonmetal Powder (NPCB) of waste printed circuit boards with phase change characteristics and a preparation method thereof.
Background
The printed circuit board is also called a printed circuit board, is manufactured by adopting an electronic printing technology, is a core component of an electronic product, is a support body of an electronic component, and is a carrier for electrically connecting the electronic component. As an indispensable component of electronic terminal equipment, the development level of the printed circuit board industry reflects the development speed and technical level of the national or regional electronic information industry to a certain extent, so that the updating speed of electronic products is improved, and electronic wastes such as waste printed circuit boards, waste parts, waste components and the like cannot be scientifically and reasonably treated, and are accumulated in a large amount, so that the electronic wastes are incinerated and landfilled, and soil pollution, water quality pollution, air pollution and even human health are caused.
In the electronic waste, the waste printed circuit board comprises a metal part and a nonmetal part, wherein the metal part accounts for about 30 percent, the nonmetal part accounts for about 70 percent, and the nonmetal part mainly comprises glass fiber, epoxy resin, phenolic resin and the like. At present, the recovery technology for the metal part is mature, but the recovery treatment and the recycling method for the nonmetal part with relatively low value are not complete temporarily, so that secondary pollution is very easy to cause, and the recovery and the utilization of the waste printed circuit nonmetal powder are necessary.
Energy is the basis for human survival and development, and as the wheel of the world economy rolls forward, the development of industrial technology is also changing. At present, fossil energy is still a main energy source, but fossil resources such as coal, natural gas and the like face the exhaustion crisis, the energy shortage gradually becomes a break-over for development of various countries, and in order to realize sustainable development, search and application of non-fossil energy such as wind energy, solar energy and the like, how to efficiently utilize limited resources, and research and development of novel energy storage materials to improve the energy utilization rate become an urgent research subject. The phase-change energy storage material stores energy by latent heat, utilizes the thermal effect in the phase-change process of the material, releases the stored energy under proper conditions, has large storable energy density and stable temperature of output energy, improves the energy utilization rate, is a green energy material, and is very important to widen the application place of the phase-change material.
Disclosure of Invention
Based on the problems, the invention aims to provide a high-filling non-metal powder (NPCB) polymer composite material with phase change property for waste printed circuit boards and a preparation method thereof, so that the NPCB can be recycled in large scale and in large batch, and the development of new energy industries can be promoted.
The high-filling NPCB polymer composite material with the phase change characteristic provided by the invention is a composite material which is nontoxic in raw materials, simple in preparation process, good in mechanical property, thermal stability and high in phase change enthalpy value, and can realize large-scale recovery of the NPCB, reduce production cost and realize resource recycling.
The object of the invention is achieved by at least one of the following technical solutions.
The preparation method of the high-filling NPCB polymer composite material with the phase change characteristic comprises the following steps:
(1) Adopting a melt blending method, uniformly mixing NPCB, a high molecular polymer, a processing aid thereof and a phase change material, and adding the mixture into an open mill for further uniform mixing to obtain a blend; the high molecular polymer is polyvinyl chloride PVC; the processing aid mainly comprises a heat stabilizer, a processing modifier, a foaming agent, a foaming aid, calcium carbonate and a plasticizer;
(2) And (3) placing the blend in the step (1) into a die by adopting a die pressing process, performing hot press forming in a hot press, and then curing in a cold press to obtain the high-filling NPCB polymer composite material with the phase change characteristic.
Further, the NPCB in the step (1) is a nonmetal part recovered from the waste printed circuit board.
Preferably, the components of the NPCB include glass fibers and a thermosetting resin; the mass ratio of the glass fiber to the thermosetting resin is 50-60:40-50.
Further, the high molecular polymer in the step (1) is polyvinyl chloride, and the brand SG5.
Further, the processing aids of the high molecular polymer in the step (1) are calcium zinc stabilizer, stearic acid, AC foaming agent, calcium carbonate, ACR530, epoxidized soybean oil and ACR401.
Further, the high-filling NPCB polymer composite material with the phase change characteristic in the step (1) is erythritol and an alloy.
Further, in the step (1), according to the parts by weight,
if calculated according to mass percent, in the blend in the step (1), the NPCB accounts for 63.75-90%, the high molecular polymer and the auxiliary agent thereof account for 11.25-30%, and the phase change material accounts for 5-15%.
Further, the temperature of the mixing in the step (1) is 160-165 ℃, preferably 160 ℃, and the mixing time is 15-20min.
Further, the hot press molding temperature in the step (2) is 170 ℃ to 175 ℃, preferably 170 ℃.
Further, the time of the hot press molding in the step (2) is 4-5min, preferably 4min.
Further, the pressure of the hot press molding in the step (2) is 9-12MPa.
Further, the curing pressure in the step (2) is 9-12MPa.
Further, the curing time in step (2) is 4-5min, preferably 4min.
Further, the curing temperature in the step (2) is normal temperature.
The invention provides a high-filling NPCB polymer composite material with phase change property, which is prepared by the preparation method.
The high-filling NPCB polymer composite material with the phase change characteristic has higher phase change enthalpy value, better thermal stability and chemical stability, no liquid phase leakage after the phase change process and good bending performance.
And the high-filling NPCB polymer composite material with the phase change characteristic greatly realizes the recovery of the NPCB, reduces the production cost, improves the resource utilization rate and has good application prospect.
The preparation method provided by the invention adopts a melt blending method and a mould pressing method, has simple preparation process, no pollution to raw materials and low cost, and is suitable for industrial production.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The preparation process is simple, the raw materials are pollution-free, the cost is low, and the preparation method is suitable for industrial production.
(2) The NPCB adopted in the invention is low-value powder which is difficult to process in industry and has great harm to environment, body and society, and is a nonmetallic material recovered from waste printed circuit boards, and the invention realizes the recycling of waste resources.
(3) The high molecular polymer adopted by the invention is polyvinyl chloride, and the filler in the composite material is well bonded together, so that the prepared plate has certain mechanical strength, can not leak liquid phase in the phase change process, and has good thermal stability and chemical stability.
(4) The phase change material used in the invention is erythritol and alloy, the phase change enthalpy value can be changed by adding the change of the erythritol with high latent heat value, the alloy with low phase change temperature mainly plays a role in enhancing mechanical properties, and the invention widens the application ideas and occasions of the erythritol and the alloy.
Drawings
FIG. 1 is a graph of flexural properties and heat distortion temperature of NPCB/PVC composites prepared in examples 1-3.
FIG. 2 is a graph of flexural performance, heat distortion temperature and DSC curve of NPCB/PVC/erythritol composites prepared in examples 4-6.
FIG. 3 is a graph of flexural performance, heat distortion temperature and DSC curve of NPCB/PVC/erythritol/alloy composites prepared in examples 7-9.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but are not intended to limit the practice and protection of the invention. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
The weight (parts by mass) used in the following examples and comparative examples may be, for example, gram, kilogram, etc., or any other amount commonly used in the art.
The NPCB used in the following examples is a nonmetallic part recovered from a waste printed circuit board. The components of the NPCB include glass fibers and a thermosetting resin; the mass ratio of the glass fiber to the thermosetting resin is 56:44.
the high molecular polymer described in the following examples is polyvinyl chloride, brand SG5, purchased from Hubei chemical industry Co., ltd.
In the following examples, the amounts of the high molecular polymer and the processing aid are as follows in parts by mass:
the phase change materials described in the following examples were purchased from Shanghai Meilin Biochemical technologies Co., ltd; the phase change material comprises erythritol and an alloy, wherein the alloy consists of 25% of lead, 12.5% of tin, 50% of bismuth and 12.5% of cadmium in percentage by mass.
Example 1
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 38g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roll open mill for mixing, and setting the temperature to 160 ℃; adding 152g of NPCB for mixing after mixing uniformly, and mixing for 18min to obtain a blend, wherein the mass ratio of NPCB/polyvinyl chloride to the auxiliary agent is 80/20;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for curing for 4min, wherein the curing pressure is 10MPa, and obtaining the NPCB/PVC composite material.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to test bending performance (according to GB/T9341-2000 "Plastic bending Performance test method"), a microcomputer-controlled thermal deformation Vicat softening point tester is used to test thermal stability (according to GB/T1634-2004 "Plastic bending load thermal deformation temperature test method").
The composite material has a flexural modulus of 9.02GPa, a flexural strength of 50.34MPa and a heat distortion temperature of 84.1 ℃. FIG. 1 is a graph of the flexural properties and heat distortion temperature of the composite material.
Example 2
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 31.5g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, adding 178.5g of NPCB, mixing for 18min to obtain a blend, wherein the mass ratio of NPCB to polyvinyl chloride to the auxiliary agent is 85/15;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for curing for 4min, wherein the curing pressure is 10MPa, and obtaining the NPCB/PVC composite material.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to test bending performance (according to GB/T9341-2000 "Plastic bending Performance test method"), a microcomputer-controlled thermal deformation Vicat softening point tester is used to test thermal stability (according to GB/T1634-2004 "Plastic bending load thermal deformation temperature test method").
The composite material has a flexural modulus of 9.51GPa, a flexural strength of 55.02MPa and a heat distortion temperature of 94.37 ℃. FIG. 1 is a graph of the flexural properties and heat distortion temperature of the composite material.
Example 3
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 21.5g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; adding 193.5g of NPCB for mixing after mixing uniformly, and mixing for 18min to obtain a blend, wherein the mass ratio of NPCB to polyvinyl chloride to the auxiliary agent is 90/10;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for curing for 4min, wherein the curing pressure is 10MPa, and obtaining the NPCB/PVC composite material.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to test bending performance (according to GB/T9341-2000 "Plastic bending Performance test method"), a microcomputer-controlled thermal deformation Vicat softening point tester is used to test thermal stability (according to GB/T1634-2004 "Plastic bending load thermal deformation temperature test method").
The composite material has a flexural modulus of 11.95GPa, a flexural strength of 58.61MPa and a heat distortion temperature of 94.37 ℃. FIG. 1 is a graph of the flexural properties and heat distortion temperature of the composite material.
Example 4
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 27.08g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, alternately adding 153.43g of NPCB and 9.5g of erythritol, mixing for 14min to obtain a blend, wherein the mass ratio of (NPCB/polyvinyl chloride/auxiliary agent)/erythritol is 95 (85/15)/5;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 12.01GPa, a flexural strength of 47.06MPa, a heat distortion temperature of 82.2 ℃, a phase transition temperature of 116.8 ℃ and a phase transition enthalpy of 5.44J/g. FIG. 2 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Example 5
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 25.65g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, alternately adding 145.35g of NPCB and 19g of erythritol, mixing for 14min to obtain a blend, wherein the mass ratio of (NPCB/polyvinyl chloride and auxiliary agent)/erythritol is 90 (85/15)/10;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 11.57GPa, a flexural strength of 31.39MPa, a heat distortion temperature of 82.9 ℃, a phase transition temperature of 118.5 ℃ and a phase transition enthalpy of 21.77J/g. FIG. 2 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Example 6
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 24.23g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, alternately adding 137.28g of NPCB and 28.5g of erythritol, mixing for 14min to obtain a blend, wherein the mass ratio of (NPCB/polyvinyl chloride/auxiliary agent)/erythritol is 85 (85/15)/15;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 10.19GPa, a flexural strength of 30.21MPa, a heat distortion temperature of 88.4 ℃, a phase transition temperature of 119.2 ℃ and a phase transition enthalpy of 40.49J/g. FIG. 2 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Example 7
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 26.78g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, and then alternately adding 151.73g of NPCB, 25.2g of erythritol and 6.3g of alloy to perform mixing, wherein the mass ratio of (NPCB/polyvinyl chloride and auxiliary agent)/(erythritol/alloy) is 85 (85/15)/15 (80/20) after mixing for 14 min;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol/alloy composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 11.84GPa, a flexural strength of 34.34MPa, a heat distortion temperature of 101.1 ℃, a phase transition temperature of 118.2 ℃ and a phase transition enthalpy of 24.21J/g. FIG. 3 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Example 8
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 26.78g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing evenly, alternately adding 151.73g of NPCB, 23.63g of erythritol and 7.88g of alloy, mixing for 14min to obtain a blend, wherein the mass ratio of (NPCB/polyvinyl chloride and auxiliary agent)/(erythritol/alloy) is 85 (85/15)/15 (75/25);
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol/alloy composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 13.94GPa, a flexural strength of 37.67MPa, a heat distortion temperature of 103.2 ℃, a phase transition temperature of 118.2 ℃ and a phase transition enthalpy of 19.73J/g. FIG. 3 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Example 9
A high-filling waste printed circuit board Nonmetal Powder (NPCB) polymer composite material with phase change characteristics and a preparation method thereof. The preparation method comprises the following steps:
(1) Weighing 26.78g of polyvinyl chloride and an auxiliary agent according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agent, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 160 ℃; mixing uniformly, and then alternately adding 151.73g of NPCB, 22.05g of erythritol and 9.45g of alloy for mixing, wherein the mass ratio of (NPCB/polyvinyl chloride and auxiliary agent)/(erythritol/alloy) is 85 (85/15)/15 (70/30) after mixing for 14 min;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for solidification, wherein the solidification time is 4min, and the solidification pressure is 10MPa, so that the NPCB/PVC/erythritol/alloy composite material (the high-filling NPCB high-molecular composite material with the phase change characteristic) is obtained.
(4) The composite material is taken out and made into standard sample bars on a universal sample making machine to carry out bending performance test (according to GB/T9341-2000 plastic bending performance test method), a microcomputer is used for controlling a thermal deformation Vicat softening point tester to carry out thermal stability test (according to GB/T1634-2004 plastic bending load thermal deformation temperature test method), a Differential Scanning Calorimeter (DSC) is used for testing phase change characteristics (according to GB/T19466.3-2004 plastic Differential Scanning Calorimeter (DSC) part 3: melting and crystallization temperature and enthalpy determination).
The composite material has a flexural modulus of 13.96GPa, a flexural strength of 39.45MPa, a heat distortion temperature of 103.4 ℃, a phase transition temperature of 118 ℃ and a phase transition enthalpy of 18.84J/g. FIG. 3 is a graph of the flexural properties, heat distortion temperature, and DSC test ramp-up period of the composite.
Comparative example 1
The macromolecule composite shaping phase change material is prepared by the following method:
(1) Weighing 40g of polyvinyl chloride and 30g of NPCB as auxiliary agents thereof according to the proportion, uniformly mixing the polyvinyl chloride and the auxiliary agents, adding the mixture into a double-roller open mill for mixing, and setting the temperature to 150 ℃; adding 30g of polyethylene glycol (with molecular weight of 2000) after uniform mixing, and mixing for 8min to obtain a blend;
(2) Placing the blend into a forming die with the thickness of 4mm, and placing the blend into a hot press for forming, wherein the hot pressing temperature is 170 ℃, the hot pressing time is 4min, and the hot pressing pressure is 10MPa;
(3) And directly placing the die subjected to hot pressing into a cold press for curing for 5min under the curing pressure of 10MPa to obtain the polyethylene glycol/polyvinyl chloride/N-PCB composite shaping phase change material.
(4) The composite material was taken out and made into standard sample bars on a universal sample machine for bending performance test (according to GB/T9341-2000 "Plastic bending Performance test method"), and the phase change characteristics thereof were tested by using a Differential Scanning Calorimeter (DSC) (according to GB/T19466.3-2004 "determination of melting and crystallization temperatures and enthalpy of plastics Differential Scanning Calorimeter (DSC) section 3).
The phase transition temperature of the composite shaped phase change material is 58.7 ℃, the phase transition enthalpy is 38.08J/g, the bending strength is 14.30MPa, and the bending modulus is 2.42GPa.
The performance tests of the composites prepared in the above groups of examples and comparative examples are shown in the following table:
table 1 effect of examples and comparative examples on composite properties
Conclusion: as can be seen from the comparison of the properties in Table 1, NPCBs in examples 1, 2 and 3 were doped to 90wt% at most, the loading was higher than that of NPCBs in comparative example 1, and the bending properties of the composite materials were also superior at this time, but the composite materials did not have phase change properties due to the absence of the phase change material. In examples 4, 5, 6, the NPCB loading is still higher than that of comparative example 1, while possessing higher bending properties and heat distortion temperature, with the exception that in example 6, the phase transition enthalpy value is also higher than that of comparative example 1. The NPCB filling amount of examples 7, 8, 9 is also higher than that of comparative example 1, and the bending property and heat distortion temperature are higher than those of examples 4, 5, 6, but the phase change enthalpy value is reduced because the enthalpy value is slightly lower than that of comparative example 1 because the phase change enthalpy value of erythritol is higher and the content of the phase change material is lower, so that an excellent composite material having high doping NPCB, low cost, high bending property, high thermal stability and phase change property can be obtained at the same time by slightly adjusting the ratio.
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.
Claims (10)
1. The preparation method of the high-filling waste printed circuit board nonmetal powder polymer composite material with the phase change characteristic is characterized by comprising the following steps of:
(1) Uniformly mixing NPCB, a high molecular polymer, a processing aid thereof and a phase change material, and carrying out open mill to obtain a blend; the high molecular polymer is polyvinyl chloride PVC; the processing aid mainly comprises a heat stabilizer, a processing modifier, a foaming agent, a foaming aid, calcium carbonate and a plasticizer;
(2) And (3) placing the blend in the step (1) in a mould, hot-pressing and molding, and then curing to obtain the high-filling NPCB polymer composite material with phase change characteristics.
2. The method for preparing the high-filling non-metal powder polymer composite material with the phase change characteristic for the waste printed circuit board according to claim 1, wherein the NPCB is a non-metal powder part recovered from the waste printed circuit board.
3. The method for preparing the high-filling waste printed circuit board nonmetal powder high-molecular composite material with the phase change property according to claim 1, wherein in the step (1), the high-molecular polymer is polyvinyl chloride (PVC);
the processing aid is calcium zinc stabilizer, stearic acid, AC foaming agent, calcium carbonate, ACR530, epoxidized soybean oil and ACR401.
4. The method for preparing the high-filling waste printed circuit board nonmetal powder polymer composite material with the phase change property according to claim 2, wherein the components of the NPCB comprise glass fibers and thermosetting resin; the mass ratio of the glass fiber to the thermosetting resin is 50-60:40-50.
5. The method for preparing the high-filling waste printed circuit board nonmetal powder polymer composite material with the phase change characteristic according to claim 1, wherein in the step (1), the phase change material is erythritol and an alloy.
6. The method for preparing the high-filling waste printed circuit board nonmetal powder polymer composite material with the phase change property according to claim 1, wherein in the step (1), according to mass fraction,
7. the method for preparing the high-filling non-metal powder polymer composite material with the phase change property of the waste printed circuit board according to claim 1, wherein in the step (1), the temperature of the front roller and the rear roller for mixing is 160-165 ℃, and the mixing time is 15-20min.
8. The method for preparing the high-filling non-metal powder polymer composite material with the phase change property of the waste printed circuit board according to claim 1, wherein in the step (2), the hot press molding temperature is 170-175 ℃, the hot press molding time is 4-5min, and the hot press molding pressure is 9-12MPa.
9. The method for preparing a high-filled NPCB polymer composite material with phase change property according to claim 1, wherein in the step (2), the curing pressure is 9-12MPa, and the curing time is 4-5min.
10. A high-filled NPCB polymer composite material having a high phase change property, produced by the production method of any one of claims 1 to 9.
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