CN113683815A - Method for lossless closed-loop recovery of carbon fibers in composite material - Google Patents
Method for lossless closed-loop recovery of carbon fibers in composite material Download PDFInfo
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- CN113683815A CN113683815A CN202110782511.3A CN202110782511A CN113683815A CN 113683815 A CN113683815 A CN 113683815A CN 202110782511 A CN202110782511 A CN 202110782511A CN 113683815 A CN113683815 A CN 113683815A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 49
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000011084 recovery Methods 0.000 title claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 39
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 39
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000003825 pressing Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000004593 Epoxy Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000004744 fabric Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000003063 flame retardant Substances 0.000 claims abstract description 8
- 150000002466 imines Chemical class 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000012958 reprocessing Methods 0.000 claims abstract description 4
- 230000015556 catabolic process Effects 0.000 claims description 13
- 238000006731 degradation reaction Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 9
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 10
- 238000012545 processing Methods 0.000 description 7
- 238000003860 storage Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940085805 fiberall Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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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
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/28—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic compounds containing nitrogen, sulfur or phosphorus
-
- 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
- C08J11/00—Recovery or working-up of waste materials
-
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- 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
Abstract
The invention discloses a method for lossless closed-loop recovery of carbon fibers in a composite material, which comprises the steps of S1, preparation of an epoxy resin solution, S2, preparation of a prepreg, S3, preparation of the composite material, S4, preparation of a cooling material, S5, carbon fiber reprocessing recovery and S6, and closed-loop recovery. The invention adopts the three-functional high-temperature resistant epoxy resin, the phosphorus-containing flame-retardant epoxy resin and the imine-containing curing agent to prepare the epoxy resin solution, then the carbon fiber cloth to be treated is subjected to the steps of dipping, drying, laying and pressing to obtain the composite material, and finally the ethylene diamine is used for degrading the composite material, so that the carbon fiber can be directly separated from the cloth without damage, and the epoxy blend EPF can be recycled after the distillation and pressing treatment, thereby realizing the repeated reutilization of the raw materials, avoiding the waste in the whole process and effectively avoiding the secondary pollution.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of carbon fiber recovery, in particular to the technical field of a method for recovering carbon fibers in a composite material in a lossless closed loop mode.
[ background of the invention ]
Carbon fiber reinforced high-performance thermosetting epoxy resin-based composite materials (CFRC) are increasingly applied to the large-scale transportation field of airplanes, automobiles, high-speed trains, ships and the like due to the advantages of high strength-to-weight ratio, high rigidity-to-weight ratio, good fatigue resistance and the like. However, the good mechanical, thermal and chemical properties of CFRC's own three-dimensional, permanently crosslinked network structure, in turn, make it difficult to recover carbon fibers therefrom.
In order to avoid waste of carbon fibers, at present, methods for recovering carbon fibers from CFRC waste mainly include a mechanical pulverization method, a chemical solvent method, a thermal cracking method, a supercritical method, and the like. These methods, while each having advantages, have disadvantages. The mechanical crushing method can only obtain the mixed scraps of the high polymer and the carbon fiber finally, and the recycling added value is extremely low. Both the thermal cracking process and the supercritical process require the use of special pressure-resistant or high-temperature-resistant devices, resulting in a significant increase in the recovery cost of the carbon fibers. The chemical solvent method may obtain a waste liquid of organic solvent or nitric acid in which polymers are dissolved after the treatment, and the treatment of the waste liquid increases the recycling cost and causes secondary pollution if the waste liquid is not properly treated. Therefore, how to recover carbon fibers from CFRC waste in a useful and non-destructive manner is a problem to be solved.
[ summary of the invention ]
The invention aims to solve the problems in the prior art and provides a lossless closed-loop method for recovering carbon fibers in a composite material, which can recover the carbon fibers from CFRC waste in a useful and lossless manner.
In order to achieve the purpose, the invention provides a method for recovering carbon fibers in a composite material in a lossless closed loop mode, which comprises the following steps:
s1, preparation of an epoxy resin solution:
weighing 6.5-8.5 parts by weight of trifunctional high-temperature-resistant epoxy resin, 6.5-8.5 parts by weight of phosphorus-containing flame-retardant epoxy resin and 6.5-10.5 parts by weight of imine-containing curing agent, mixing the trifunctional high-temperature-resistant epoxy resin and the phosphorus-containing flame-retardant epoxy resin to obtain an epoxy blend EPF, adding the imine-containing curing agent, and mixing to obtain an epoxy resin solution;
s2, preparation of prepreg:
soaking the carbon fiber cloth to be recovered into the epoxy resin solution prepared in the step S1, taking out the carbon fiber cloth soaked with the epoxy resin solution, and drying to obtain a prepreg;
s3, preparation of the composite material:
laying the prepreg layers prepared in the S2 layer by layer, and then pressing and curing at high temperature to obtain a composite material;
s4, preparing a cooling material:
cooling the composite material prepared in the step S3 to obtain a cooling material;
s5, carbon fiber reprocessing and recycling:
putting the prepared cooling material in S4 into excessive Ethylenediamine (EDA) and heating until complete degradation to obtain degradation liquid and carbon fiber, and cleaning and drying the carbon fiber;
s6, closed loop recovery:
distilling the degradation liquid prepared in S5 under vacuum to obtain recycled epoxy powder, and pressing the epoxy powder to obtain the epoxy blend EPF.
Preferably, in S1, the trifunctional refractory epoxy resin is MF-3101L epoxy resin.
Preferably, in the step S2, the drying temperature is 60-100 ℃, and the drying time is 10-20 mins.
Preferably, in the S3, the pressing pressure is 0.1-0.3 MPa, the curing is carried out for 40-80 mins in three sections, and the curing temperature in the three sections is 60-100 ℃, 120-160 ℃ and 150-190 ℃.
Preferably, in the S4, the composite material prepared in the S3 is cooled to 20-30 ℃.
Preferably, in S5, the degradation temperature is 80-120 ℃, and the degradation time is 1.5-2.5 h.
Preferably, in the S6, the pressing temperature is 160-200 ℃, the pressing pressure is 4-6 MPa, and the pressing time is 20-60 mins.
The invention has the beneficial effects that: the preparation method comprises the steps of preparing a trifunctional high-temperature-resistant epoxy resin, a phosphorus-containing flame-retardant epoxy resin and an imine-containing curing agent together to form an epoxy resin solution, then carrying out the steps of dipping, drying, laying and pressing on carbon fiber cloth to be treated to obtain a composite material, finally degrading the composite material by using ethylenediamine, directly and nondestructively separating carbon fibers from the cloth, recovering an epoxy blend EPF after distillation and pressing treatment, realizing the repeated reutilization of raw materials, avoiding waste in the whole process and effectively avoiding secondary pollution; through cooling the composite material, the viscosity between the fiber cloth is improved and the fiber cloth is solidified, so that the shaping effect of the fiber cloth is improved.
The features and advantages of the present invention will be described in detail by embodiments in conjunction with the accompanying drawings.
[ description of the drawings ]
FIG. 1 is a partial schematic flow chart of the first embodiment;
FIG. 2 is a SEM image of example II.
In the figure: a-CFRC of 50 μm grade before processing; b-20 μm class CFRC before processing; c-CFRC of 50 μm grade after two successive processes; d-CFRC of 20 μm grade after two consecutive processes.
[ detailed description ] embodiments
The first embodiment is as follows:
s1, preparation of an epoxy resin solution:
weighing 7.5g parts of trifunctional high-temperature-resistant epoxy resin, 7.5g parts of phosphorus-containing flame-retardant epoxy resin and 8.7 parts of imine-containing curing agent in parts by weight, mixing the trifunctional high-temperature-resistant epoxy resin and the phosphorus-containing flame-retardant epoxy resin to obtain an epoxy blend EPF, adding the imine-containing curing agent, and mixing to obtain an epoxy resin solution;
wherein the trifunctional high-temperature-resistant epoxy resin is MF-3101L epoxy resin;
s2, preparation of prepreg:
soaking the carbon fiber cloth to be recovered into the epoxy resin solution prepared in the step S1, taking out the carbon fiber cloth soaked with the epoxy resin solution, and drying to obtain a prepreg;
wherein the drying temperature is 80 ℃, and the drying time is 15 mins;
s3, preparation of the composite material:
laying the prepreg layers prepared in the S2 layer by layer, and then pressing and curing at high temperature to obtain a composite material;
wherein, the curing is carried out for 60mins in three sections under the pressing pressure of 0.2MPa, and the curing temperature in the three sections is respectively 80 ℃, 140 ℃ and 170 ℃;
s4, preparing a cooling material:
cooling the composite material prepared in the step S3 to obtain a cooling material;
wherein the composite prepared in S3 is cooled to 25 ℃;
s5, carbon fiber reprocessing and recycling:
putting the prepared cooling material in S4 into excessive ethylenediamine, heating until the cooling material is completely degraded to obtain degradation liquid and carbon fibers, and cleaning and drying the carbon fibers;
wherein the degradation temperature is 100 ℃, and the degradation time is 2 h;
s6, closed loop recovery:
distilling the degradation liquid prepared in the S5 under vacuum to obtain recycled epoxy powder, and pressing the epoxy powder to obtain an epoxy blend EPF;
wherein the pressing temperature is 180 ℃, the pressing pressure is 5MPa, and the pressing time is 40 mins.
Example two:
the carbon fiber reinforced high-performance thermosetting epoxy resin-based composite material (CFRC) was continuously processed twice as in example, and various physical properties of the carbon fiber recovered before processing and after each processing were measured, and the test results are shown in table 1 below:
| sample name | Storage modulus (MPa) | Tensile Strength (MPa) | Flexural strength (Mpa) |
| Starting material | 2964 | 705 | 603 |
| Is processed once | 3478 | 625 | 564 |
| Processing twice | 3801 | 578 | 490 |
TABLE 1 physical Properties of carbon fibers
Referring to fig. 1 and 2, after one processing, the storage modulus of the recycled carbon fiber increased by 17.34%, and the tensile strength and the flexural strength were decreased by 11.35% and 6.47%, respectively, while after two processing, the storage modulus of the recycled carbon fiber increased by 28.24%, and the tensile strength and the flexural strength were decreased by 18.01% and 18.74%, respectively. After being processed once or twice, the storage modulus, tensile strength and bending strength of the recycled carbon fiber all meet the recycling standard. In addition, scanning electron microscopy showed that the surface of the carbon fibers before and after recovery did not change much.
The above embodiments are illustrative of the present invention, and are not intended to limit the present invention, and any simple modifications of the present invention are within the scope of the present invention.
Claims (7)
1. A method for lossless closed-loop recovery of carbon fibers in a composite material is characterized by comprising the following steps:
s1, preparation of an epoxy resin solution:
weighing 6.5-8.5 parts by weight of trifunctional high-temperature-resistant epoxy resin, 6.5-8.5 parts by weight of phosphorus-containing flame-retardant epoxy resin and 6.5-10.5 parts by weight of imine-containing curing agent, mixing the trifunctional high-temperature-resistant epoxy resin and the phosphorus-containing flame-retardant epoxy resin to obtain an epoxy blend EPF, adding the imine-containing curing agent, and mixing to obtain an epoxy resin solution;
s2, preparation of prepreg:
soaking the carbon fiber cloth to be recovered into the epoxy resin solution prepared in the step S1, taking out the carbon fiber cloth soaked with the epoxy resin solution, and drying to obtain a prepreg;
s3, preparation of the composite material:
laying the prepreg layers prepared in the S2 layer by layer, and then pressing and curing at high temperature to obtain a composite material;
s4, preparing a cooling material:
cooling the composite material prepared in the step S3 to obtain a cooling material;
s5, carbon fiber reprocessing and recycling:
putting the prepared cooling material in S4 into excessive ethylenediamine, heating until the cooling material is completely degraded to obtain degradation liquid and carbon fibers, and cleaning and drying the carbon fibers;
s6, closed loop recovery:
distilling the degradation liquid prepared in S5 under vacuum to obtain recycled epoxy powder, and pressing the epoxy powder to obtain the epoxy blend EPF.
2. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: in the S1, the trifunctional high-temperature-resistant epoxy resin is MF-3101L epoxy resin.
3. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: and in the step S2, the drying temperature is 60-100 ℃, and the drying time is 10-20 mins.
4. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: in the S3, the pressing pressure is 0.1-0.3 MPa, three sections are respectively solidified for 40-80 mins, and the three sections are respectively solidified at the temperatures of 60-100 ℃, 120-160 ℃ and 150-190 ℃.
5. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: and in the S4, cooling the composite material prepared in the S3 to 20-30 ℃.
6. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: in the S5, the degradation temperature is 80-120 ℃, and the degradation time is 1.5-2.5 h.
7. A method of lossless, closed-loop carbon fiber recovery in composites, as claimed in claim 1, wherein: in the S6, the pressing temperature is 160-200 ℃, the pressing pressure is 4-6 MPa, and the pressing time is 20-60 mins.
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| CN202110782511.3A CN113683815B (en) | 2021-07-12 | 2021-07-12 | Method for recovering carbon fibers in composite material in lossless closed-loop mode |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| CN103524784A (en) * | 2012-05-04 | 2014-01-22 | 艾达索高新材料无锡有限公司 | Degrading and recovering method of epoxy resin composite material |
| CN109206646A (en) * | 2018-08-14 | 2019-01-15 | 艾达索高新材料芜湖有限公司 | A kind of degradable epoxy chopped carbon fiber felt prepreg and its production technology |
| CN109320918A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院宁波材料技术与工程研究所 | Recyclable carbon-fibre reinforced epoxy resin composite material, preparation method and application |
-
2021
- 2021-07-12 CN CN202110782511.3A patent/CN113683815B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| CN103524784A (en) * | 2012-05-04 | 2014-01-22 | 艾达索高新材料无锡有限公司 | Degrading and recovering method of epoxy resin composite material |
| CN109206646A (en) * | 2018-08-14 | 2019-01-15 | 艾达索高新材料芜湖有限公司 | A kind of degradable epoxy chopped carbon fiber felt prepreg and its production technology |
| CN109320918A (en) * | 2018-11-07 | 2019-02-12 | 中国科学院宁波材料技术与工程研究所 | Recyclable carbon-fibre reinforced epoxy resin composite material, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| CHRISTIANE SALES REIS DE SOUZA等: ""Reuse of Uncured Carbon Fiber/Epoxy Resin Prepreg Scraps: Mechanical Behavior and Environmental Response"", 《ACS SUSTAINABLE CHEMISTRY & ENGINEERING》, vol. 7, pages 2200 - 2206, XP055658757, DOI: 10.1021/acssuschemeng.8b04852 * |
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