CN110922677A - Preparation process and detection method of microcapsule toughening and reinforcing polypropylene composite material - Google Patents
Preparation process and detection method of microcapsule toughening and reinforcing polypropylene composite material Download PDFInfo
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- CN110922677A CN110922677A CN201911252544.6A CN201911252544A CN110922677A CN 110922677 A CN110922677 A CN 110922677A CN 201911252544 A CN201911252544 A CN 201911252544A CN 110922677 A CN110922677 A CN 110922677A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 123
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 111
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 103
- 239000002131 composite material Substances 0.000 title claims abstract description 69
- -1 polypropylene Polymers 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000003014 reinforcing effect Effects 0.000 title claims abstract description 14
- 238000001514 detection method Methods 0.000 title claims abstract description 8
- 239000002775 capsule Substances 0.000 claims abstract description 49
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000002156 mixing Methods 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000012545 processing Methods 0.000 claims abstract description 14
- 229920001807 Urea-formaldehyde Polymers 0.000 claims abstract description 13
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims abstract description 13
- 238000005469 granulation Methods 0.000 claims abstract description 6
- 230000003179 granulation Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 39
- 239000011162 core material Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 20
- 239000000839 emulsion Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 239000004202 carbamide Substances 0.000 claims description 17
- 239000008098 formaldehyde solution Substances 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 14
- 239000003822 epoxy resin Substances 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000009864 tensile test Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000002296 dynamic light scattering Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000004580 weight loss Effects 0.000 claims description 5
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- 238000000576 coating method Methods 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 238000000518 rheometry Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000004626 scanning electron microscopy Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000002787 reinforcement Effects 0.000 claims 2
- 238000010979 pH adjustment Methods 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 19
- 230000004048 modification Effects 0.000 abstract description 19
- 229920005989 resin Polymers 0.000 abstract description 7
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- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 235000011149 sulphuric acid Nutrition 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
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- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000002715 modification method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000742679 Coprosma repens Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 101100223811 Caenorhabditis elegans dsc-1 gene Proteins 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- 229910052906 cristobalite Inorganic materials 0.000 description 1
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- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- FOUWCSDKDDHKQP-UHFFFAOYSA-N flumioxazin Chemical compound FC1=CC=2OCC(=O)N(CC#C)C=2C=C1N(C1=O)C(=O)C2=C1CCCC2 FOUWCSDKDDHKQP-UHFFFAOYSA-N 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- 235000009566 rice Nutrition 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/006—Crack, flaws, fracture or rupture
- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a preparation process and a detection method of a microcapsule toughening and reinforcing polypropylene composite material, which are characterized by comprising the following steps of firstly, preparing an ST-UF microcapsule by taking Styrene (ST) as a capsule core and urea-formaldehyde resin (UF) as a capsule wall; and then, mixing the polypropylene/microcapsule composite material, adding 3-5 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass parts, mixing, and then carrying out mixing granulation to obtain the polypropylene/microcapsule composite material. The invention has the advantages that the ST-UF microcapsule is introduced into PP resin, the processing performance of PP can be obviously improved, the preparation process of the ST-UF microcapsule is not complicated, but the ST-UF microcapsule can obviously improve the strength, toughness and processing fluidity of PP after being used for PP modification, and a certain repairability is also endowed; in addition, the ST-UF microcapsule has good thermal stability and shear resistance, completely meets the processing condition requirements of PP materials, and does not cause adverse effects on the processing and use of PP.
Description
Technical Field
The invention belongs to the technical field of polypropylene composite material preparation, and particularly relates to a preparation process and a detection method of a microcapsule toughening and reinforcing polypropylene composite material.
Background
The molecular chain of polypropylene (PP) has three configurations of isotactic, syndiotactic and atactic, the industrial product mainly has isotactic and syndiotactic, and the PP has high crystallinity and exists mainly in the form of spherulite because of the good structural regularity of the molecular chain. This makes PP have good mechanical strength, corrosion resistance, heat resistance, but also have the disadvantages of poor low temperature impact resistance and easy aging. Therefore, the modification of PP materials has been an important issue in the field of PP applications.
The PP modification comprises chemical modification and physical modification, and the physical modification method mainly comprises the following steps: filling modification, reinforcing modification, blending modification, nanoparticle modification and the like. The various modification methods are roughly as follows: 1) and (5) filling modification. Inorganic filler or organic filler is added into PP resin, so that the cost is reduced as a main purpose, certain physical properties of the PP, such as heat resistance, degradation property and the like, can be improved, and mica powder, calcium carbonate, wollastonite, wood powder, rice hull powder, corn cob core and the like are commonly used; 2) and (4) enhancing modification. The modification mainly aims at increasing the strength of PP, and the reinforced materials mainly comprise glass fibers, asbestos fibers, single crystal fibers and the like; 3) and (4) blending modification. Mainly means that other polymers of a second component such as plastics, rubber or thermoplastic elastomers are introduced into a PP matrix, so that the strength, toughness and low-temperature brittleness of the PP are improved. 4) And (4) modifying the nano particles. The purpose of toughening and strengthening PP is realized by inducing PP rapid crystallization and PP/nanoparticle two-phase interface effect through nanoparticles, and the commonly used nanoparticles comprise nano SiO2, nano Al2O3, nano TiO2 and the like. In the various physical modification methods, the key points of modification are the induction of PP crystallization and the exertion of interface effect, and the invention aims to provide a novel preparation process for improving the processing performance of PP and repairing microcracks.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation process and a detection method of a microcapsule toughening and reinforcing polypropylene composite material, wherein an ST-UF microcapsule which takes Styrene (ST) as a capsule core and urea-formaldehyde resin (UF) as a capsule wall is prepared and used for PP modification to prepare the polypropylene/microcapsule composite material.
In order to realize the aim, the invention adopts the technical scheme that the preparation process of the microcapsule toughening and reinforcing polypropylene composite material comprises the following steps of firstly, preparing ST-UF microcapsules by taking Styrene (ST) as a capsule core and urea-formaldehyde resin (UF) as a capsule wall; and then, mixing the polypropylene/microcapsule composite material, adding 3-5 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass parts, mixing, and then carrying out mixing granulation to obtain the polypropylene/microcapsule composite material.
Further, the ST-UF microcapsule is prepared by the following steps:
step 1), urea and formaldehyde solution are weighed according to the mass ratio of 10: 18-22 and mixed, the pH value of the system is adjusted to 7-8, and then the mixture is stirred to react to obtain a capsule wall prepolymer;
step 2), weighing 100 parts of styrene, 30-40 parts of epoxy resin, 4-5 parts of acetone and 30-40 parts of tributyl phosphate according to the mass part ratio, uniformly stirring, adding 180-200 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2-3 parts of n-octanol, and continuously stirring for 25-30 min at 30 ℃ and 500-800 rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
step 3), coating the capsule core by the capsule wall: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the stirring condition, adjusting the pH value of the system to be 3-4, filtering with filter paper after stirring reaction, then dissolving and washing with distilled water and ethanol, and drying the obtained product to obtain the ST-UF microcapsule.
Further, triethanolamine is adopted in the step 1) to adjust the pH value of the system, and then the system is stirred and reacted for 1 hour in a constant-temperature water bath kettle at the temperature of 70-75 ℃ to obtain the capsule wall prepolymer.
Further, the reaction vessel of the step 2) is a three-neck flask.
Further, dilute H is used in the step 3)2SO4And adjusting the pH value of the system.
Further, in the step 3), the stirring reaction is carried out at 50 ℃ for 1.5-2 h at 500-800 rpm; dissolving and washing the mixture for 3 times by using distilled water and ethanol respectively in the step 3).
Further, when the polypropylene/microcapsule composite material is mixed, a three-section single-screw extruder is adopted for mixing and granulation after mixing.
Further, the three-section temperature of a screw of the three-section single-screw extruder is respectively 165-180 ℃, 200-210 ℃ and 190-200 ℃; the die temperature was set as: 190-200 ℃; the rotating speed of the screw is set as follows: 15-25 r/min; can effectively prevent the microcapsules from breaking under the action of high temperature and shearing.
The invention also provides a detection method of the microcapsule toughened and reinforced polypropylene composite material, which comprises the self-repairing capability test of the composite material, and comprises the following specific steps: selecting 6 uniform samples from the tensile samples with the same components, and performing tensile test on 3 samples according to the national standard, wherein the national standard condition is that the room temperature is 20 ℃, the tensile speed is 50mm/min, and the average values of the tensile strength and the elongation at break are obtained; taking the average value of the tensile strength as the average tensile strength, stretching the other 3 samples to 70% of the average tensile strength under the national standard condition, terminating the stretching, then placing the samples in an oven at 80 ℃ for 24h, and performing the tensile test under the national standard condition again to obtain the average values of the tensile strength and the elongation at break as the data after the material is repaired, thereby judging the self-repairing capability of the polypropylene/microcapsule composite material.
Further, the method also comprises the steps of testing the ST-UF microcapsule by dynamic light scattering, Fourier transform infrared spectroscopy, a scanning electron microscope and thermal weight loss, and analyzing the particle size, the functional group structure, the micro morphology and the sealing property of the microcapsule; and testing the torque rheology, the stretching and the repairability of the polypropylene/microcapsule composite material, and analyzing the processing performance and the mechanical performance of the composite material.
Compared with the prior art, the invention has at least the following beneficial effects that the invention creatively provides the component formula and the coating process of the microcapsule and the blending process of the polypropylene/microcapsule composite material, the ST-UF microcapsule which takes Styrene (ST) as a capsule core and urea-formaldehyde resin (UF) as a capsule wall is used for PP modification to prepare the polypropylene/microcapsule composite material, and in the composite material system, the ST-UF microcapsule is dispersed in a PP matrix and can be used as a crystal nucleus to improve the crystallization rate of a PP molecular chain, so that PP crystal grains are refined; meanwhile, when the PP generates micro-cracks under the action of external force, the micro-capsules are torn by the expanded micro-cracks with a certain probability, and ST monomers overflowing from the micro-cracks are closed by the self-aggregation, so that the micro-cracks are prevented from further expanding.
Furthermore, the microcapsule and the PP resin are both organic materials, so that the interface combination is firmer; a small amount of ST-UF microcapsules are added into PP resin, so that the toughening and strengthening effects on PP can be effectively realized, and the service life of PP can be prolonged;
furthermore, the ST-UF microcapsule is introduced into PP resin, so that the processing performance of PP can be obviously improved, the preparation process of the ST-UF microcapsule is not complicated, but the ST-UF microcapsule can obviously improve the strength, toughness and processing fluidity of PP after being used for PP modification, and a certain repairability is endowed; in addition, the ST-UF microcapsule has good thermal stability and shear resistance, completely meets the processing condition requirements of PP materials, and does not cause adverse effects on the processing and use of PP.
Drawings
FIG. 1 is a scanning electron micrograph of ST-UF microcapsules.
FIG. 2 is a scanning electron microscope image of the tensile section of the polypropylene/microcapsule composite material.
Detailed Description
The invention will be further described with reference to the drawings and the detailed description, but the invention is not limited to the following examples.
Materials, reagents and apparatus for use in the invention
1) The main materials and reagents used are as follows:
urea, analytically pure, six chemical reagents factories of Tianjin;
formaldehyde solution (37%), chemical purity, Chengduo chemical reagent factory;
triethanolamine, analytically pure, remote chemical reagents ltd, tianjin;
styrene, analytically pure, jiao zhou futian chemical reagent factory;
epoxy resin (E-44), technical grade, Lanzhou Lanxing resin, Inc.;
acetone, analytically pure, eastern red chemical plant, guangzhou city;
tributyl phosphate, analytically pure, shinyleaf and refinish fine chemical research institute of Tianjin;
sodium dodecyl benzene sulfonate, analytically pure, shinyleaf and refinish chemical research institute of Tianjin;
n-octanol, analytically pure, red rock reagent factory in eastern river, Tianjin;
concentrated sulfuric acid (H)2SO4) Chemically pure, zinc industries, llc in hanzhong;
absolute ethanol, chemical purity, sienna sanpu fine chemical plant;
PP powder, KL0058-2002, Clarityiene chemical Co, China.
2) The used equipment mainly comprises:
electronic balance, VALOR 3000, shanghai asian limited;
a drying oven, DHG-9146A, shanghai essence macro laboratory instruments ltd;
dynamic Light Scattering (DLS), Nano ZS-90, Malvern, UK;
a fourier transform infrared spectrometer, Nicolet 6700, Nicolet corporation, usa;
thermogravimetric analyzer (TG), DSC-1, METTLER TOLEDO (Shanghai) instruments, Inc.;
particle size analyzer, RISE-2008, science and technology Limited of Jinan Run;
torque rheometer, Polylab QC, HAAKE, germany;
tensile testing machine, LDS-20KN, Intelligent testing machine research institute of Changchun city;
scanning Electron Microscope (SEM), SU8010, Hitachi corporation, japan;
scanning Electron Microscopy (SEM), JSM-6390LV, JEOL Inc., Japan;
in addition, there are conventional laboratory facilities such as beakers, flasks, three-necked flasks, water baths, and the like.
Example 1:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:18, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 8 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 74 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 37 parts of epoxy resin, 4 parts of acetone and 39 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 188 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2 parts of n-octanol, and continuously stirring for 27min at 30 ℃ and 750rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 3 by using dilute H2SO4, reacting for 2 hours at the temperature of 50 ℃ and the speed of 800rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 3 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 165 ℃, 210 ℃, 190 ℃ and 195 ℃; the screw speed may be set as: 15 r/min.
Detection of polypropylene/microcapsule composite material:
1) testing the ST-UF microcapsule by dynamic light scattering, Fourier transform infrared spectroscopy, a scanning electron microscope and thermal weight loss, and analyzing the particle size, the functional group structure, the micro morphology and the sealing property of the microcapsule;
2) testing the torque rheology, the stretching and the repairability of the polypropylene/microcapsule composite material, and analyzing the processing performance, the mechanical performance and the self-repairing capability of the composite material;
3) the self-repairing capability test method of the composite material is designed by the invention, and comprises the following specific operations: selecting 6 uniform samples from the tensile samples with the same components, and performing tensile test on 3 samples according to national standards to obtain average values of tensile strength and elongation at break; and stretching the other 3 samples to 70% of the average tensile strength under the national standard condition, then terminating the stretching, then placing the samples in an oven at 80 ℃ for 24h, and performing the stretching test under the national standard condition again to obtain the average values of the tensile strength and the elongation at break as data after the material is repaired, so as to judge the self-repairing capability of the polypropylene/microcapsule composite material, wherein the national standard condition is 20 ℃ at room temperature and 50mm/min at the stretching speed, and the stretching test under the national standard condition is a preferred embodiment of the invention, and the stretching test of the invention can be performed at the same room temperature and stretching speed.
Example 2:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:21, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 7 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 73 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 30 parts of epoxy resin, 5 parts of acetone and 38 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 185 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2.5 parts of n-octanol, and continuously stirring for 26min at the temperature of 30 ℃ and the speed of 500rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 3 by using dilute H2SO4, reacting for 1.8H under the conditions of 50 ℃ and 550rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 3.5 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 175 ℃, 203 ℃, 193 ℃ and 193 ℃; the screw speed may be set as: 17 r/min.
Example 3:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:20, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 7 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 75 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 35 parts of epoxy resin, 4 parts of acetone and 40 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 190 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2 parts of n-octanol, and continuously stirring for 27min at the conditions of 30 ℃ and 600rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 4 by using dilute H2SO4, reacting for 1.5H under the conditions of 50 ℃ and 600rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 4 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 170 ℃, 205 ℃, 200 ℃ and 195 ℃; the screw speed may be set as: 20 r/min.
Example 4:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:21, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 8 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 70 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 40 parts of epoxy resin, 4.5 parts of acetone and 30 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 195 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 3 parts of n-octanol, and continuously stirring for 28min at the conditions of 30 ℃ and 550rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 4 by using dilute H2SO4, reacting for 1.7H under the conditions of 50 ℃ and 700rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 4 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 168 deg.C, 202 deg.C, 197 deg.C; the screw speed may be set as: 22 r/min.
Example 5:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:18, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 7 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 72 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 32 parts of epoxy resin, 5 parts of acetone and 31 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 198 parts of sodium dodecyl benzene sulfonate aqueous solution with the concentration of 1% and 2.5 parts of n-octanol, and continuously stirring for 25min at the temperature of 30 ℃ and the speed of 800rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 4 by using dilute H2SO4, reacting for 2 hours at the temperature of 50 ℃ and the speed of 750rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 5 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 178 ℃, 208 ℃, 192 ℃ and 192 ℃; the screw speed may be set as: 23 r/min.
Example 6:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:22, adding the urea and the formaldehyde solution into a flask, adjusting the pH value of the system to be 7 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 70 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 32 parts of epoxy resin, 4 parts of acetone and 39 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 188 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 3 parts of n-octanol, and continuously stirring for 30min at 30 ℃ and 750rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 3 by using dilute H2SO4, reacting for 1.5H under the conditions of 50 ℃ and 650rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 4 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 165 ℃, 200 ℃; the screw speed may be set as: 25 r/min.
Example 7:
preparation of ST-UF microcapsules:
1) weighing urea and formaldehyde solution according to the mass ratio of 10:19, adding the urea and formaldehyde solution into a flask, adjusting the pH value of the system to be 7.5 by using triethanolamine, then putting the flask into a constant-temperature water bath kettle at 71 ℃, and stirring for reacting for 1h to obtain a capsule wall prepolymer;
2) weighing 100 parts of styrene, 30 parts of epoxy resin, 5 parts of acetone and 35 parts of tributyl phosphate according to the mass part ratio, adding the weighed materials into a three-neck flask, fully and uniformly stirring, adding 200 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2 parts of n-octanol, and continuously stirring for 30min at the temperature of 30 ℃ and the speed of 750rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
3) the capsule wall covers the capsule core: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the condition of stirring, adjusting the pH value of the system to be 3 by using dilute H2SO4, reacting for 1.7H under the conditions of 50 ℃ and 500rpm, filtering by using filter paper, dissolving and washing for 3 times by using distilled water and ethanol respectively, and drying the obtained product to obtain the ST-UF microcapsule.
The blending process of the polypropylene/microcapsule composite material comprises the following steps: adding 3 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass part ratio, simply mixing, and then mixing and granulating by adopting a three-section single-screw extruder to obtain a polypropylene/microcapsule composite material; the three-stage temperature and the die temperature of the screw may be set to: 180 ℃, 205 ℃, 195 ℃ and 200 ℃; the screw speed may be set as: 18 r/min.
The structure and performance of the ST-UF microcapsule and the polypropylene/microcapsule composite material of the invention
FIG. 1 shows a scanning electron micrograph of ST-UF microcapsules, and it can be seen that the size of a single capsule is about 5 μm, the size is uniform, but a sticky structure exists, and the dynamic light scattering average particle size is about 9 μm.
Meanwhile, the infrared spectrum result shows that the characteristic peak C-N, C ═ O, N-H of the urea-formaldehyde resin, the characteristic peak benzene ring and C ═ C of the styrene resin and the characteristic peak-O-of the epoxy resin exist, and the microcapsules are respectively washed by water and ethanol for 3 times, so that the result can prove that the styrene and the epoxy resin are coated in the microcapsules; the thermal weight loss result shows that the thermal weight loss is concentrated in two ranges of 240-310 ℃ and 350-420 ℃, namely monomer volatilization after the microcapsules are broken and thermal decomposition of urea-formaldehyde resin, and the breaking temperature of the microcapsules is higher than the processing temperature of PP, so that the microcapsules completely meet the temperature requirements of PP modification and material use.
FIG. 2 is a scanning electron microscope image of a tensile section of a polypropylene/microcapsule composite, and it can be seen that a considerable amount of microcapsules remain intact and uniformly dispersed in a PP matrix after melting, shear mixing, granulation and tensile testing. As can be seen from FIG. 2, the polypropylene/microcapsule composite material has uneven tensile section and exhibits obvious ductile fracture characteristics
Meanwhile, torque rheological tests show that compared with pure PP materials, after the composite material is modified by the microcapsules, the change of the non-Newtonian index of the composite material is not large, but the Newtonian viscosity constant is reduced to about 50% of the original value, and the processing fluidity of the composite material is obviously improved. Tensile test shows that the tensile strength of the composite material is improved by about 15 percent, the elongation at break is improved by about 50 percent, and the urea-formaldehyde resin microcapsule has good toughening and reinforcing effects on PP. The repairability test shows that after the composite material sample strip is pre-stretched and repaired, the average tensile strength of the composite material sample strip is about 110% of that before the composite material sample strip is repaired, and the microcapsule has a repairing and reinforcing effect on the damage of the PP matrix.
When ST-UF microcapsules can be prepared, the stirring speed is increased or decreased to obtain microcapsules with smaller or larger particle size; the core of the microcapsule can adopt other similar material formulas; ST-UF microcapsules can be used for the modification of other types of polymeric materials.
The details of the present invention not described in detail are prior art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation process of a microcapsule toughening and reinforcing polypropylene composite material is characterized by comprising the following steps of firstly, preparing ST-UF microcapsules by taking Styrene (ST) as a capsule core and urea-formaldehyde resin (UF) as a capsule wall; and then, mixing the polypropylene/microcapsule composite material, adding 3-5 parts of ST-UF microcapsules into 100 parts of PP powder according to the mass parts, mixing, and then carrying out mixing granulation to obtain the polypropylene/microcapsule composite material.
2. The preparation process of the microcapsule toughening and reinforcing polypropylene composite material according to claim 1, wherein the ST-UF microcapsule is prepared by the following steps:
step 1), urea and formaldehyde solution are weighed according to the mass ratio of 10: 18-22 and mixed, the pH value of the system is adjusted to 7-8, and then the mixture is stirred to react to obtain a capsule wall prepolymer;
step 2), weighing 100 parts of styrene, 30-40 parts of epoxy resin, 4-5 parts of acetone and 30-40 parts of tributyl phosphate according to the mass part ratio, uniformly stirring, adding 180-200 parts of 1% sodium dodecyl benzene sulfonate aqueous solution and 2-3 parts of n-octanol, and continuously stirring for 25-30 min at 30 ℃ and 500-800 rpm to form a stable oil-in-water (O/W) emulsified solution, namely a core material emulsion;
step 3), coating the capsule core by the capsule wall: adding the capsule wall prepolymer solution prepared in the step 1) into the core material emulsion under the stirring condition, adjusting the pH value of the system to be 3-4, filtering with filter paper after stirring reaction, then dissolving and washing with distilled water and ethanol, and drying the obtained product to obtain the ST-UF microcapsule.
3. The preparation process of the microcapsule toughening and reinforcement polypropylene composite material according to claim 2, wherein triethanolamine is used for system pH adjustment in the step 1), and then the microcapsule toughening and reinforcement polypropylene composite material is stirred and reacted for 1 hour in a constant-temperature water bath kettle at 70-75 ℃ to obtain a capsule wall prepolymer.
4. The process for preparing the microcapsule toughened and reinforced polypropylene composite material as claimed in claim 2, wherein the reaction vessel of the step 2) is a three-neck flask.
5. The process for preparing the polypropylene composite material toughened and reinforced by the microcapsules according to claim 2, wherein dilute H is used in the step 3)2SO4And adjusting the pH value of the system.
6. The preparation process of the microcapsule toughening and reinforcing polypropylene composite material according to claim 2, wherein the parameters of the stirring reaction in the step 3) are that the reaction is carried out for 1.5-2 h at 50 ℃ and 500-800 rpm; dissolving and washing the mixture for 3 times by using distilled water and ethanol respectively in the step 3).
7. The process for preparing the microcapsule toughened and reinforced polypropylene composite material according to claim 1, wherein the polypropylene/microcapsule composite material is blended and then mixed by a three-stage single screw extruder for granulation.
8. The preparation process of the microcapsule toughening and reinforcing polypropylene composite material according to claim 7, wherein the three-section temperature of the screw of the three-section single screw extruder is 165-180 ℃, 200-210 ℃ and 190-200 ℃ respectively; the die temperature was set as: 190-200 ℃; the rotating speed of the screw is set as follows: 15 to 25 r/min.
9. A detection method for a microcapsule toughening and reinforcing polypropylene composite material is characterized by comprising a self-repairing capability test of the composite material, and comprises the following specific steps: selecting 6 uniform samples from the tensile samples with the same components, performing tensile test on 3 samples according to the national standard, wherein the national standard condition is that the room temperature is 20 ℃, the tensile speed is 50mm/min, obtaining the average values of the tensile strength and the elongation at break, taking the average value of the tensile strength as the average tensile strength, stopping the tensile after the other 3 samples are stretched to 70% of the average tensile strength under the national standard condition, then placing the samples in an oven at 80 ℃ for 24h, performing the tensile test under the national standard condition again, obtaining the average values of the tensile strength and the elongation at break as the data after the material is repaired, and judging the self-repairing capability of the polypropylene/microcapsule composite material.
10. The method for detecting the microcapsule toughened and reinforced polypropylene composite material according to claim 9, further comprising the steps of testing the ST-UF microcapsules by dynamic light scattering, Fourier transform infrared spectroscopy, scanning electron microscopy and thermal weight loss, and analyzing the particle size, the functional group structure, the micro morphology and the sealing property of the microcapsules; and testing the torque rheology, the stretching and the repairability of the polypropylene/microcapsule composite material, and analyzing the processing performance and the mechanical performance of the composite material.
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| CN102492174A (en) * | 2011-11-30 | 2012-06-13 | 哈尔滨工业大学 | Urea resin wrapped dicyclopentadiene nanometer microcapsule, and synthetic method and application thereof |
| KR20120118274A (en) * | 2011-04-18 | 2012-10-26 | 주식회사 폴리사이언텍 | Scratch self-healing polypropylene composition and mouldings produced therefrom |
| CN107353592A (en) * | 2017-07-05 | 2017-11-17 | 奇瑞汽车股份有限公司 | A kind of selfreparing carbon fibre composite part and preparation method thereof |
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| KR20120118274A (en) * | 2011-04-18 | 2012-10-26 | 주식회사 폴리사이언텍 | Scratch self-healing polypropylene composition and mouldings produced therefrom |
| CN102492174A (en) * | 2011-11-30 | 2012-06-13 | 哈尔滨工业大学 | Urea resin wrapped dicyclopentadiene nanometer microcapsule, and synthetic method and application thereof |
| CN107353592A (en) * | 2017-07-05 | 2017-11-17 | 奇瑞汽车股份有限公司 | A kind of selfreparing carbon fibre composite part and preparation method thereof |
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